反应 #2139951

ord-fb0d8d027bae4846bae619fed066a54b

反应方程式

CCCCCC1CCC(c2ccc3c(c2F)c(=O)oc2c(F)c(OCCCC)ccc23)CC1
3-butoxy-4,7-difluoro-8-(4-pentylcyclohexyl)-benzo[c]chromen-6-one
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
Lawesson's reagent
CCCCCC1CCC(c2ccc3c(c2F)c(=S)oc2c(F)c(OCCCC)ccc23)CC1
3-butoxy-4,7-difluoro-8-(4-pentylcyclohexyl)benzo[c]chromene-6-thione
收率 65.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The solution was subsequently filtered through silica gel
  2. 2
    其他evaporated
  3. 3
    其他the crude product was purified by crystallisation from MTB ether

实验过程

11.7 g (25.6 mmol) of 3-butoxy-4,7-difluoro-8-(4-pentylcyclohexyl)-benzo[c]chromen-6-one and 11.4 g (28.2 mmol) of Lawesson's reagent were refluxed for 16 hours in 130 ml of chlorobenzene. The solution was subsequently filtered through silica gel and evaporated, and the crude product was purified by crystallisation from MTB ether, giving 7.9 g (65%) of 3-butoxy-4,7-difluoro-8-(4-pentylcyclohexyl)benzo[c]chromene-6-thione as yellow crystals.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07326447B2uspto-grants-2008_02