反应 #217017

ord-07e4f8c57880493e91f3b448105bb0cd

反应方程式

CCOC(=O)C(=O)OCC
diethyl oxalate
CC(=O)c1nccs1
acetylthiazole
CCOC(=O)C(=O)CC(=O)c1nccs1
2,4-diketo-4-(thiazol-2-yl)butyric acid ethyl ester
收率 72.2%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added dropwise
  2. 2
    浓缩concentrated
  3. 3
    workup.ADDITIONThe residue was treated with 100 ml of water and neutralized with 6N HCl
  4. 4
    过滤Filtration

实验过程

To a sodium ethoxide solution (prepared from 150 ml of ethanol and 4.2 g of sodium) at 0° C., a mixture of diethyl oxalate (22.98 g) and acetylthiazole (20.07 g) was added dropwise. The resulting mixture was stirred at room temperature for 2 hours and concentrated. The residue was treated with 100 ml of water and neutralized with 6N HCl. Filtration afforded 25.8 g of 2,4-diketo-4-(thiazol-2-yl)butyric acid ethyl ester as brown solids. NMR: 1.46 (t, 3H), 4.49 (q, 2H), 7.27 (s, 1H), 7.65, 8.04 (2d, 2H, thiazolyl H's).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05470862uspto-grants-1995_11