Water → Methyl 4-cyano-3-oxobutanoate
反応式
[C-:1]#[N:2].[K+].Cl[CH2:5][C:6](=[O:12])[CH2:7][C:8]([O:10][CH3:11])=[O:9].O>CO.S(=O)(=O)(O)O>[C:1]([CH2:5][C:6](=[O:12])[CH2:7][C:8]([O:10][CH3:11])=[O:9])#[N:2]参加物
6
反応条件
- 温度
- 40 °C
実験手順
After 0.4 g of potassium cyanide was added at room temperature to a solution of 1 g of Methyl 4-chloro-3-oxobutanoate in 20 ml of methanol, the resulting mixture was warmed to 40° C. and maintained for further 8 hours. Thereafter, reaction solution was cooled and pH of the solution was adjusted to 3 by adding 10 ml of water and a few drops of concentrated sulfuric acid. After the mixture was extracted thrice with diethyl ether, total amount of which was 100 ml, the separated organic layers were combined and concentrated under reduced pressure to give 0.6 g of methyl 4-cyano-3-oxobutanoate (Purity: 71%).
後処理
- temperaturemaintained for further 8 hours
- customThereafter, reaction solution
- temperaturewas cooled
- extractionAfter the mixture was extracted thrice with diethyl ether, total amount of which
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0bbd713c8be34d339bac4ee9bd7ed0f1
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06781009B2
反応ノート
読み込み中…