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Hydrazinecarboxylic acid, ethyl ester → N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| 反応物 | 2-Cyclopropylacetaldehyde | HCID 10307849 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N'-(2-Cyclopropylethylidene)hydrazinecarboxylic acid ethyl ester | HCID 69310105 | 85% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425552B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-4b3a774da7f34e66bb4f679f126c9102 |
| 出典メモ | uspto-grants-2008_09 |