1-氨基-3,6,9-三噁-11-十一醇

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a one-liter 3-necked flask equipped with a thermometer, stirrer, dropping funnel and a nitrogen inlet was 122 g (0.5M) of TMXDI (from American Cyanamid). Then 193 g (1.0 mole) of tetraethylene glycol monoamine was added over a 50 minute period keeping the temperature below 36° C. A clear viscous product was obtained. To a one-liter 3-necked flask equipped with a thermometer, stirrer the temperature below 36° C A clear viscous product was obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound VII (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound VII (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of Compound XXV (15.94 g; 72.7 mmole) in 100 ml of pyridine was added triphenylphosphine (29 g; 111 mmole). After stirring for one hour, at which time gas evolution had subsided, 50 ml of concentrated aqueous ammonium hydroxide was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2). The aqueous layer was washed twice with 200 ml ether each time. The aqueous layer was adjusted to pH 11 with solid sodium hydroxide and extracted three times with 150 ml n-butanol each time. The butanol extract was dried over sodium sulfate, filtered and concentrated. The residue was taken up in tetrahydrofuran and filtered. The filtrate was evaporated to a syrup which was azeotroped with toluene. the mixture stirred overnight The reaction mixture was concentrated under vacuum the residue partitioned between 200 ml of water and 200 ml of ether (aqueous layer at pH 2) The aqueous layer was washed twice with 200 ml ether each time extracted three times with 150 ml n-butanol each time The butanol extract was dried over sodium sulfate filtered concentrated filtered The filtrate was evaporated to a syrup which was azeotroped with toluene