反应 #2139917

ord-3354a96ad0934a8b8256b541dc25fbd1

反应方程式

CNC(=S)NN
4-methyl-3-thiosemicarbazide
CC(C)=O
acetone
CC(=O)CCl
chloroacetone
CC(C)=NN=c1scc(C)n1C
3,4-Dimethyl-2(3H)-thiazolone-(1-methylethyliden) hydrazone

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux for 2 hours
  2. 2
    温度The reaction mixture was heated
  3. 3
    温度at reflux for 7 hours
  4. 4
    浓缩concentrated
  5. 5
    其他The resulting crude product was recrystallized from acetone

实验过程

21 g (200 mmol) of 4-methyl-3-thiosemicarbazide in 1000 mL of acetone was heated at reflux for 2 hours. To the solution was then added dropwise 20.4 g (220 mmol) of chloroacetone. The reaction mixture was heated at reflux for 7 hours and concentrated. The resulting crude product was recrystallized from acetone. This gave 23 g of an orange powder (63% of the theoretical).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07326254B2uspto-grants-2008_02