反应 #80967

ord-a7eb556908204482bceb93a605ec7ad7

反应方程式

CC(C)C(N)=S
2-methylpropane-thioamide
O=C(CCl)CCl
1,3-dichloroacetone
O=S(=O)([O-])[O-].[Mg+2]
MgSO4
CC(C)c1nc(CCl)cs1.Cl
crude desired compound
CC(C)c1nc(CCl)cs1.Cl
4-(Chloromethyl)-2-isopropylthiazole hydrochloride

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 3.5 h
  3. 3
    温度to cool
  4. 4
    过滤filtered
  5. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616720uspto-grants-1997_04