Benzyl isocyanate → ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetate

HRID 576875노트

반응식

HRID 576875 반응식
[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH2:3].[CH2:10]([N:17]=[C:18]=[O:19])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O1CCCC1.C(OCC)(=O)C>[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH:3][C:18](=[O:19])[NH:17][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

5

반응물 2

HCID 76639Benzyl isocyanateHCID 20288078Ethyl 2-(1-methylhydrazinyl)acetate

생성물 1

HCID 66977957ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetate수율 76%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of ethyl 2-(1-methylhydrazinyl)acetate (Compound XL-1) 10 ml (76 mmol) in tetrahydrofuran 40 ml, benzyl isocyanate 11.1 g (83.3 mmol) was added at 0° C. and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate 150 ml and washed with water 75 ml and brine 75 ml. The organic phase was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to obtain the title compound 15.2 g (76%).

후처리

  1. washwashed with water 75 ml and brine 75 ml
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-e456841d45a84c60b5e7cea3ed743214
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040531B2

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