1,1,1-三氟-3-吗啉-4-基丙-2-醇

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

实验步骤: In a round bottomed reaction vessel, under argon, was placed 0.239 g (1.2 mmol) of 1,1,1-trifluoro-3-morpholin-4-yl-propan-2-ol and 0.203 g (1.3 mmol) of 4-chlorophenyl isocyanate. The vessel was capped, set in a bath at 85° C. and stirred. After 90 min, the mixture was cooled. The crude material was purified by chromatography on silica gel, eluting with hexanes-ethyl acetate (90:10), to give 0.250 g (59%) of (4-chloro-phenyl)-carbamic acid 2,2,2-trifluoro-1-morpholin-4-ylmethyl-ethyl ester as a white crystalline solid. (M+H)+=353 m/e. In a round bottomed reaction vessel, under argon, was placed The vessel was capped set in a bath at 85° C. the mixture was cooled The crude material was purified by chromatography on silica gel eluting with hexanes-ethyl acetate (90:10)

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

实验步骤: In a round bottomed reaction vessel, under argon, was placed 0.239 g (1.2 mmol) of 1,1,1-trifluoro-3-morpholin-4-yl-propan-2-ol and 0.203 g (1.3 mmol) of 4-chlorophenyl isocyanate. The vessel was capped, set in a bath at 85° C. and stirred. After 90 min, the mixture was cooled. The crude material was purified by chromatography on silica gel, eluting with hexanes-ethyl acetate (90:10), to give 0.250 g (59%) of (4-chloro-phenyl)-carbamic acid 2,2,2-trifluoro-1-morpholin-4-ylmethyl-ethyl ester as a white crystalline solid. (M+H)+=353 m/e. In a round bottomed reaction vessel, under argon, was placed The vessel was capped set in a bath at 85° C. the mixture was cooled The crude material was purified by chromatography on silica gel eluting with hexanes-ethyl acetate (90:10)

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

实验步骤: To a round bottomed flask containing 3.136 g (36 mmol) of morpholine was added 3.362 g (30 mmol) of racemic 1,1,1-trifluoro-2,3-epoxypropane dropwise over 10 min (exothermic). The mixture was stirred at room temperature. After 90 min, the volatiles were removed under reduced pressure to give 5.837 g (98%) of 1,1,1-trifluoro-3-morpholin-4-yl-propan-2-ol as an oil. the volatiles were removed under reduced pressure

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

实验步骤: In a round bottomed reaction vessel, under argon, was placed 0.239 g (1.2 mmol) of 1,1,1-trifluoro-3-morpholin-4-yl-propan-2-ol and 0.203 g (1.3 mmol) of 4-chlorophenyl isocyanate. The vessel was capped, set in a bath at 85° C. and stirred. After 90 min, the mixture was cooled. The crude material was purified by chromatography on silica gel, eluting with hexanes-ethyl acetate (90:10), to give 0.250 g (59%) of (4-chloro-phenyl)-carbamic acid 2,2,2-trifluoro-1-morpholin-4-ylmethyl-ethyl ester as a white crystalline solid. (M+H)+=353 m/e. In a round bottomed reaction vessel, under argon, was placed The vessel was capped set in a bath at 85° C. the mixture was cooled The crude material was purified by chromatography on silica gel eluting with hexanes-ethyl acetate (90:10)

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

实验步骤: To a round bottomed flask containing 3.136 g (36 mmol) of morpholine was added 3.362 g (30 mmol) of racemic 1,1,1-trifluoro-2,3-epoxypropane dropwise over 10 min (exothermic). The mixture was stirred at room temperature. After 90 min, the volatiles were removed under reduced pressure to give 5.837 g (98%) of 1,1,1-trifluoro-3-morpholin-4-yl-propan-2-ol as an oil. the volatiles were removed under reduced pressure