反応 #45213

反応方程式

2-Cyano-N-(1,1-dimethylethyl)-2-[(diphenylmethylene)amino]acetamide

ethyl acetate

HCl

→

2-amino-2-cyano-N-(1,1-dimethylethyl)-acetamide hydrochloride

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他equipped with a nitrogen inlet, a gas outlet tube
2. 2
   温度reflux condenser
3. 3
   温度thermometer, mechanical stirrer, and maintained under a positive pressure of nitrogen
4. 4
   温度gradually cooled to room temperature
5. 5
   その他) The resulting layers were separated
6. 6
   抽出the aqueous phase was extracted with CH2Cl2 (4 L)
7. 7
   抽出The combined organic solutions were extracted with aqueous HCl (1N, 2×0.5 L)
8. 8
   濃縮concentrated under reduced pressure

実験手順

2-Cyano-N-(1,1-dimethylethyl)-2-[(diphenylmethylene)amino]acetamide 4 (900 g, 2.818 mol), ethyl acetate (4.5 L) and aqueous HCl (1 N. 4.5 L) were placed into a 12 L three-necked flask equipped with a nitrogen inlet, a gas outlet tube, reflux condenser, thermometer, mechanical stirrer, and maintained under a positive pressure of nitrogen. The mixture was heated on an oil bath at 60° C. for 4 hours with vigorous stirring, gradually cooled to room temperature, and then slowly diluted with CH2Cl2 (4 L). (Thin layer chromatography (EtOAc/hexanes=1/4) indicated no more starting material was present.) The resulting layers were separated and the aqueous phase was extracted with CH2Cl2 (4 L). The combined organic solutions were extracted with aqueous HCl (1N, 2×0.5 L). The aqueous extracts were combined and concentrated under reduced pressure to yield 490 g (2.557 mol) of 2-amino-2-cyano-N-(1,1-dimethylethyl)-acetamide hydrochloride 5.HCl.

出典