反应 #80967
ord-a7eb556908204482bceb93a605ec7ad7
反应方程式
2-methylpropane-thioamide
1,3-dichloroacetone
MgSO4
→
crude desired compound
4-(Chloromethyl)-2-isopropylthiazole hydrochloride
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度was heated
- 2温度at reflux for 3.5 h
- 3温度to cool
- 4过滤filtered
- 5其他the solvent was removed in vacuo
实验过程
A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.