反応 #48756

反応方程式

(2R,5R)-2-cyclohexylmethoxy-5-[(1S,2S)-3-(3,5-difluorophenyl)-2-((E)-3-dipropylcarbamoyl-2-methylacryloylamino)-1-hydroxypropyl]-morpholine-4-carboxylic acid tert-butyl ester

hydrogen chloride

diethyl ether

→

title compound

収率 97.3%

(2R,5R)-2-Cyclohexylmethoxy-5-[(1S,2S)-3-(3,5-difluorophenyl)-2-((E)-3-dipropylcarbamoyl-2-methylacryloylamino)-1-hydroxypropyl]-morpholine-4-carboxylic acid hydrochloride

収率 97.3%

溶媒

trifluoroacetic acid

dichloromethane

反応条件

後処理

1. 1
   濃縮concentrate
2. 2
   workup.DISSOLUTIONdissolve in ethyl acetate (30 mL)
3. 3
   洗浄wash with 1:1 saturated aqueous sodium chloride
4. 4
   乾燥saturated aqueous sodium bicarbonate (30 mL), dry (sodium sulfate)
5. 5
   濃縮concentrate
6. 6
   workup.DISSOLUTIONDissolve the residue in ethyl acetate
7. 7
   濃縮concentrate

実験手順

Dissolve (2R,5R)-2-cyclohexylmethoxy-5-[(1S,2S)-3-(3,5-difluorophenyl)-2-((E)-3-dipropylcarbamoyl-2-methylacryloylamino)-1-hydroxypropyl]-morpholine-4-carboxylic acid tert-butyl ester (0.051 g, 0.075 mmol) in trifluoroacetic acid (1.5 mL) and stir at room temperature for 15 minutes. Dilute with dichloromethane (15 mL), concentrate, dissolve in ethyl acetate (30 mL), wash with 1:1 saturated aqueous sodium chloride:saturated aqueous sodium bicarbonate (30 mL), dry (sodium sulfate) and concentrate. Dissolve the residue in ethyl acetate and add 1 M hydrogen chloride in diethyl ether (0.20 mL, 0.20 mmol) and concentrate to give the title compound (0.045 g, 97.3%).

出典