1-ethoxy-2,2,3,3,3-pentafluoropropan-1-ol

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled in an argon atmosphere to −60° C. Sodium borohydride (2.16 g, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled in an argon atmosphere to −60° C. Sodium borohydride (2.16 g, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled in an argon atmosphere to −60° C. Sodium borohydride (2.16 g, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained

反応条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step. After the addition was held below −45° C The mixture was cooled to −60° C. remained below −45° C The mixture was slowly warmed to room temperature extracted with diethylether (3×100 ml) The combined organic phases were washed with water (two times) dried over magnesium sulfate the solvent was removed under reduced pressure 9.76 g (50.3 mmol, 88%) were obtained