反应 #312613

反应方程式

1-phenylsulfonyl-4-(4-benzylpiperazin-1-yl)-1H-indazole

1-chloroethyl chloroformate

→

title compound

收率 63.0%

1-(Phenylsulfonyl)-4-(1-piperazinyl)-1H-indazole hydrochloride

收率 63.0%

溶剂

1,2-dichloroethane

反应条件

后处理

1. 1
   温度heated
2. 2
   温度at reflux temperature for 2 hr
3. 3
   浓缩concentrated in vacuo
4. 4
   温度The resultant residue is heated
5. 5
   温度at reflux temperature in methanol for 1.5 hr
6. 6
   温度cooled
7. 7
   浓缩concentrated in vacuo
8. 8
   其他The resulting tan solid is triturated with ether
9. 9
   其他crystallized from hot ethanol

实验过程

A solution of 1-phenylsulfonyl-4-(4-benzylpiperazin-1-yl)-1H-indazole (433 mg, 1.0 mmol) in 1,2-dichloroethane is treated with 1-chloroethyl chloroformate (0.27 mL, 2.5 mmol) heated at reflux temperature for 2 hr, and concentrated in vacuo. The resultant residue is heated at reflux temperature in methanol for 1.5 hr, cooled, concentrated in vacuo and reconcentrated from ether. The resulting tan solid is triturated with ether and crystallized from hot ethanol to give the title compound as a tan solid 237 mg (63% yield), mp 203-205° C., identified by HNMR and mass spectral analyses.

来源