6-amino- Hexanoic acid, phenylmethyl ester, hydrochloride (1:1)

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

实验步骤: To a solution of (5R,9R)-9-(dodecanoyloxy)-1-(9H-fluoren-9-yl)-3,12-dioxo-2,11-dioxa-7-thia-4-azatricosane-5-carboxylic acid (6, 1 eq) in DMF (0.2 M) was added DIEA (5 eq) and EDCI (1.3 eq) and HOBT (1.3 eq). The reaction was stirred at room temperature for 10 minutes, which was followed by adding benzyl 6-aminohexanoate hydrochloride (1.2 eq). The reaction mixture was then stirred at room temperature overnight. The mixture was diluted with ethyl acetate, and washed with saturated NaHCO3 solution, water and brine. The organic layer was dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5% MeOH/DCM to give the title product. The reaction mixture was then stirred at room temperature overnight washed with saturated NaHCO3 solution, water and brine The organic layer was dried over anhydrous Na2SO4 concentrated en vaccuo The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO)

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

实验步骤: To a solution of (5R,9R)-9-(dodecanoyloxy)-1-(9H-fluoren-9-yl)-3,12-dioxo-2,11-dioxa-7-thia-4-azatricosane-5-carboxylic acid (6, 1 eq) in DMF (0.2 M) was added DIEA (5 eq) and EDCI (1.3 eq) and HOBT (1.3 eq). The reaction was stirred at room temperature for 10 minutes, which was followed by adding benzyl 6-aminohexanoate hydrochloride (1.2 eq). The reaction mixture was then stirred at room temperature overnight. The mixture was diluted with ethyl acetate, and washed with saturated NaHCO3 solution, water and brine. The organic layer was dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5% MeOH/DCM to give the title product. The reaction mixture was then stirred at room temperature overnight washed with saturated NaHCO3 solution, water and brine The organic layer was dried over anhydrous Na2SO4 concentrated en vaccuo The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO)

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

实验步骤: To a solution of benzyl 6-(tert-butoxycarbonylamino)hexanoate (1 eq) in DCM (0.17 M) was added 4M HCl in dioxane (30 eq). The resulting mixture was stirred at room temperature for 1 hour. The mixture was concentrated en vaccuo. The crude material was dissolved in DCM and precipitated in diethyl ether to give the product as a white solid. The mixture was concentrated en vaccuo The crude material was dissolved in DCM precipitated in diethyl ether

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

实验步骤: To a solution of benzyl 6-(tert-butoxycarbonylamino)hexanoate (1 eq) in DCM (0.17 M) was added 4M HCl in dioxane (30 eq). The resulting mixture was stirred at room temperature for 1 hour. The mixture was concentrated en vaccuo. The crude material was dissolved in DCM and precipitated in diethyl ether to give the product as a white solid. The mixture was concentrated en vaccuo The crude material was dissolved in DCM precipitated in diethyl ether

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

实验步骤: To a solution of (5R,9R)-9-(dodecanoyloxy)-1-(9H-fluoren-9-yl)-3,12-dioxo-2,11-dioxa-7-thia-4-azatricosane-5-carboxylic acid (6, 1 eq) in DMF (0.2 M) was added DIEA (5 eq) and EDCI (1.3 eq) and HOBT (1.3 eq). The reaction was stirred at room temperature for 10 minutes, which was followed by adding benzyl 6-aminohexanoate hydrochloride (1.2 eq). The reaction mixture was then stirred at room temperature overnight. The mixture was diluted with ethyl acetate, and washed with saturated NaHCO3 solution, water and brine. The organic layer was dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5% MeOH/DCM to give the title product. The reaction mixture was then stirred at room temperature overnight washed with saturated NaHCO3 solution, water and brine The organic layer was dried over anhydrous Na2SO4 concentrated en vaccuo The crude mixture was purified by flash chromatography on a COMBIFLASH® system (ISCO)

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

实验步骤: To a solution of benzyl 6-(tert-butoxycarbonylamino)hexanoate (1 eq) in DCM (0.17 M) was added 4M HCl in dioxane (30 eq). The resulting mixture was stirred at room temperature for 1 hour. The mixture was concentrated en vaccuo. The crude material was dissolved in DCM and precipitated in diethyl ether to give the product as a white solid. The mixture was concentrated en vaccuo The crude material was dissolved in DCM precipitated in diethyl ether