Hydrazinecarboxylic acid, ethyl ester → N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester

HRID 30981

반응식

HRID 30981 반응식
[CH:1]1([CH2:4][CH:5]=O)[CH2:3][CH2:2]1.[C:7]([O:11][CH2:12][CH3:13])(=[O:10])[NH:8][NH2:9]>CCO>[CH2:12]([O:11][C:7]([NH:8][N:9]=[CH:5][CH2:4][CH:1]1[CH2:2][CH2:3]1)=[O:10])[CH3:13]

참가 물질

4

반응물 2

HCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 103078492-Cyclopropylacetaldehyde

생성물 1

HCID 69310105N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester수율 85%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The solution of 2-cyclopropylethanal was diluted with 50 mL EtOH. Ethyl carbazate (5.14 g, 49.3 mmol) was added and the solution stirred at room temperature for 12 h, upon which it was concentrated in vacuo and the crude material was purified by flash column chromatography (0-5% MeOH in CH2Cl2) to give 7.1 g (85%) of the hydrazone (4a) as a colorless crystalline solid. 1H-NMR (400 MHz, CDCl3): 8.21 (br s, 1H); 7.21 (s, 1H); 4.23 (m, 2H); 2.17 (t, 3H, J=5.9 Hz) 1.06 (m, 2H); 0.80 (m, 1H); 0.1 (d, 2H); 0.48 (m, 2H); 0.13 (m, 2H) ppm.

후처리

  1. concentrationwas concentrated in vacuo
  2. customthe crude material was purified by flash column chromatography (0-5% MeOH in CH2Cl2)

출처 및 근거

ORD 기록
ord-4b3a774da7f34e66bb4f679f126c9102
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425552B2

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