Triethylamine → Ethyl 2-(1-methyl-2-(thiophen-2-ylmethylcarbamoyl)hydrazinyl)acetate

HRID 1254480노트

반응식

HRID 1254480 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH:7][C:8](=[O:19])OC1C=CC([N+]([O-])=O)=CC=1.[CH3:20][N:21]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[NH2:22].C(N(CC)CC)C>ClCCl.C(OCC)(=O)C>[CH3:20][N:21]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[NH:22][C:8](=[O:19])[NH:7][CH2:6][C:2]1[S:1][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 20288078Ethyl 2-(1-methylhydrazinyl)acetateHCID 670755344-Nitrophenyl thiophen-2-ylmethylcarbamate

생성물 1

HCID 67088516Ethyl 2-(1-methyl-2-(thiophen-2-ylmethylcarbamoyl)hydrazinyl)acetate수율 46.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To the solution of 4-nitrophenyl thiophen-2-ylmethylcarbamate (Compound XII-1) 3.14 g (11 mmol) in dichloromethane 20 ml, ethyl 2-(1-methylhydrazinyl)acetate (Compound XV-2) 2.98 g (22.6 mmol) and triethylamine 2.36 ml (17 mmol) was added at 0° C. and stirred at additional 4.5 hours. The reaction mixture was diluted with ethyl acetate 100 ml and washed with water 10 ml and brine 75 ml. The organic phase was dried with magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The residue was submitted to silcagel chromatography to obtain the title compound 1.38 g (45%).

후처리

  1. washwashed with water 10 ml and brine 75 ml
  2. dry with materialThe organic phase was dried with magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-9f5ca75a34e44eedab4fb836d3ec2571
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455488B2

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