Water → (2R)-N-methyl-2-methylamino-3-(thiophen-2-yl)propionamide

HRID 495855노트

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HRID 495855 반응식
C(O[C:6](=O)[N:7](C)[C@@H:8]([C:15](=[O:18])[NH:16][CH3:17])[CH2:9][C:10]1[S:11][CH:12]=[CH:13][CH:14]=1)(C)(C)C.FC(F)(F)C(O)=O.O.C(=O)([O-])O.[Na+]>C(Cl)Cl>[CH3:17][NH:16][C:15](=[O:18])[C@H:8]([NH:7][CH3:6])[CH2:9][C:10]1[S:11][CH:12]=[CH:13][CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 10494327N-Methyl-N-((1R)-1-(methylcarbamoyl)-2-(thiophen-2-yl)ethyl)carbamic acid tert-butylester

생성물 1

HCID 10535973(2R)-N-methyl-2-methylamino-3-(thiophen-2-yl)propionamide수율 90.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

N-Methyl-N-((1R)-1-(methylcarbamoyl)-2-(thiophen-2-yl)ethyl)carbamic acid tert-butylester (1.17 g; 3.92 mmol) was dissolved in methylene chloride (4 ml). The reaction was cooled to 0° C. and triflouroacetic acid was added. The mixture was stirred at room temperature for 1.5 hour. Water (30 ml) and solid sodium hydrogencarbonate were added to pH 8. The phases were separated. The aqueous phase was extracted with methylene chloride (4×20 ml). The combined organic phases were dried over magnesium sulfate and the solvent was removed over vacuo to afford 0.70 g of (2R)-N-methyl-2-methylamino-3-(thiophen-2-yl)propionamide.

후처리

  1. customThe phases were separated
  2. extractionThe aqueous phase was extracted with methylene chloride (4×20 ml)
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. customthe solvent was removed over vacuo

출처 및 근거

ORD 기록
ord-585a53a6517d43fb866f437e3a05261e
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939880B2

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