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HRID73597

反应详情

EQUATION

反应方程式

HRID 73597 的结构方程式

REACTANTS

反应物

2
结构：NC(=O)c1c(F)cccc1F
HCID87439

Benzamide, 2,6-difluoro-

C7H5F2NO

结构：COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
HCID87949

p-Anisyldithiophosphonic anhydride

C14H14O2P2S4

PRODUCTS

生成物

1
结构：NC(=S)c1c(F)cccc1F
HCID12683212

未命名化合物

收率 99%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

A solution of 2, 6 difluorobenzamide (1 eq) and Lawesson's reagent (0.5 eq.) in toluene (0.2 M) was heated at 90° C. for 14 hours. Upon cooling the volatiles were removed in vacuo and purified by SiO2 chromatography (25% EtOAc/hexanes) yielding 2,6-difluorobenzothioamide as a light yellow solid (99%). LCMS (m/z): 174.1 (MH+); LC Rt=2.19 min.

WORKUP

后处理

  1. temperatureUpon cooling the volatiles
  2. customwere removed in vacuo
  3. custompurified by SiO2 chromatography (25% EtOAc/hexanes)