تفاعل #80976

معادلة التفاعل

1,3-dichloroacetone

N,N-dimethylthiourea

MgSO4

→

desired compound

المردود 70.0%

4-(Chloromethyl)-2-(dimethylamino)thiazole

المردود 70.0%

المذيبات

acetone

acetone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةto reflux
3. 3
   درجة الحرارةThe resulting mixture was heated
4. 4
   درجة الحرارةat reflux for 1.5 h
5. 5
   درجة الحرارةto cool
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated in vacuo
8. 8
   أخرىThe residue was purified by silica gel chromatography

الإجراء التجريبي

A mixture of 15 g (144 mmol) of N,N-dimethylthiourea and excess MgSO4 in 350 ml of acetone was heated to reflux and treated dropwise with a solution of 18.3 g (144 mmol) of 1,3-dichloroacetone in 35 ml of acetone. The resulting mixture was heated at reflux for 1.5 h, allowed to cool, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography using 20% ethyl acetate in hexane to provide 14.0 g (70%) of the desired compound.

المصدر