반응 #48756

반응 방정식

(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

수율 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

수율 97.3%

용매

trifluoroacetic acid

dichloromethane

반응 조건

후처리

1. 1
   농축concentrate
2. 2
   workup.DISSOLUTIONdissolve in ethyl acetate (30 mL)
3. 3
   세척wash with 1:1 saturated aqueous sodium chloride
4. 4
   건조saturated aqueous sodium bicarbonate (30 mL), dry (sodium sulfate)
5. 5
   농축concentrate
6. 6
   workup.DISSOLUTIONDissolve the residue in ethyl acetate
7. 7
   농축concentrate

실험 절차

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%).

출처