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

HRID 30981

反応式

HRID 30981 の反応式
[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

反応物 2

HCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 103078492-Cyclopropylacetaldehyde

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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

  1. concentrationwas concentrated in vacuo
  2. 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

関連ノート

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