Hydrazinecarboxylic acid, ethyl ester → N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester
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
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
- concentrationwas concentrated in vacuo
- 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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