تفاعل #48756

معادلة التفاعل

(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

المردود 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

المردود 97.3%

المذيبات

trifluoroacetic acid

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%).

المصدر