반응 #652417

반응 방정식

methylamine hydrochloride

triethylamine

(2S)-2-tert-butoxycarbonylamino-3,3-dimethylbutanoic acid

→

(2S)-2-tert-butoxycarbonylamino-3,3-dimethylbutanoic acid methylamide

수율 100.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction is stirred for an additional 18 h
2. 2
   세척washed with 1 M hydrochloric acid and saturated aqueous sodium chloride
3. 3
   건조The organic layer is dried over anhydrous magnesium sulfate
4. 4
   농축concentrated in vacuo

실험 절차

To a solution of (2S)-2-tert-butoxycarbonylamino-3,3-dimethylbutanoic acid (120 g, 519 mmol) in dichloromethane (800 mL) is added 1,1-carbonyldiimidazole (88.4 g, 545 mmol). The resulting solution is stirred at 25° C. for 1 h and methylamine hydrochloride (52.5 g, 779 mmol) and triethylamine (157.3 g, 1557 mmol) are added and the reaction is stirred for an additional 18 h. The mixture is diluted with dichloromethane (600 mL) and washed with 1 M hydrochloric acid and saturated aqueous sodium chloride. The organic layer is dried over anhydrous magnesium sulfate and concentrated in vacuo to provide (2S)-2-tert-butoxycarbonylamino-3,3-dimethylbutanoic acid methylamide as a white solid (126 g, 100% yield).

출처