Hydrazinecarboxylic acid, ethyl ester → N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester
反応式
[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]参加物
4
実験手順
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.
後処理
- concentrationwas concentrated in vacuo
- customthe crude material was purified by flash column chromatography (0-5% MeOH in CH2Cl2)
出典と根拠
- ORDレコード
- ord-4b3a774da7f34e66bb4f679f126c9102
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425552B2
反応ノート
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