反应 #71070

反应方程式

amino-thioxo-acetic acid ethyl ester

1,3-dichloro-propan-2-one

EtOAc

N2

→

title compound

4-Chloromethyl-thiazole-2-carboxylic acid ethyl ester

溶剂

toluene

反应条件

后处理

1. 1
   温度at reflux
2. 2
   洗涤the mixture was washed with sat. aq. NaHCO3 (10 mL)
3. 3
   干燥The organic layer was dried over MgSO4
4. 4
   过滤filtered
5. 5
   其他the solvent removed under reduced pressure
6. 6
   其他Purification of the residue by FC (4:1 hept-EA)

实验过程

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of amino-thioxo-acetic acid ethyl ester (2.50 g, 18.77 mmol) and 1,3-dichloro-propan-2-one (2.88 g, 21.59 mmol) in toluene (20.0 mL) was stirred for 2 h at reflux. EtOAc (20 mL) was added at rt and the mixture was washed with sat. aq. NaHCO3 (10 mL) followed by brine (20 mL). The organic layer was dried over MgSO4, filtered, and the solvent removed under reduced pressure. Purification of the residue by FC (4:1 hept-EA) gave the title compound as a light yellow oil. TLC:rf (4:1 hept-EA)=0.26. LC-MS-conditions 02: tR=0.89 min, [M+H]+=206.40.

来源