反应 #45207

ord-39517b344c2c4d5c9cb17949702d5cad

反应方程式

Cc1nc2ccccc2s1
2-methylbenzothiazole
O=S1(=O)CCCCO1
1,4-butane sultone
Cc1nc2c(CCCCS(=O)(=O)O)cccc2s1
Compound 1
收率 98.1%
Cc1nc2c(CCCCS(=O)(=O)O)cccc2s1
4-(Sulfobutyl)-2-methylbenzothiazole
收率 98.1%

反应条件

温度
135°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to cool to room temperature
  2. 2
    其他the resulting mass was triturated with ethyl acetate (50 ml) until a gray solid
  3. 3
    其他separated
  4. 4
    其他The solid was collected by centrifugation
  5. 5
    洗涤washed with ethyl acetate
  6. 6
    其他dried under vacuum

实验过程

A mixture of 2-methylbenzothiazole (1.49 g, 10 mmol) and 1,4-butane sultone (4.0 g, 30 mmol) was heated in a pressure tube at 130-140° C. for 3 hours. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with ethyl acetate (50 ml) until a gray solid separated. The solid was collected by centrifugation, washed with ethyl acetate and dried under vacuum to yield 2.8 g (96%) of Compound 1.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737281B2uspto-grants-2010_06