反応 #10355

反応方程式

4,6-Dichloro-5-(2-methoxy-phenoxy)-2-methylsulfanyl-pyrimidine

benzylsulfamic acid amide potassium salt

citric acid

→

benzylsulfamic acid [6-chloro-5-(2-methoxy-phenoxy)-2-methylsulfanyl-pyrimidin-4-yl]-amide

収率 79.2%

溶媒

DMSO

反応条件

後処理

1. 1
   workup.ADDITIONThe reaction mixture was poured onto water
2. 2
   ろ過the precipitate was filtered off
3. 3
   その他purified by column chromatography over silica gel with hexane/EtOAc=2/1

実験手順

4,6-Dichloro-5-(2-methoxy-phenoxy)-2-methylsulfanyl-pyrimidine (1.5 g) was dissolved in DMSO (30 ml) and benzylsulfamic acid amide potassium salt (2.12 g, Referential Example 22) was added. Stirring was continued for 18 h. The reaction mixture was poured onto water, acidified by solid citric acid (1.9 g), cooled to 0° C. and the precipitate was filtered off and purified by column chromatography over silica gel with hexane/EtOAc=2/1 to give benzylsulfamic acid [6-chloro-5-(2-methoxy-phenoxy)-2-methylsulfanyl-pyrimidin-4-yl]-amide (1.75 g) as a white powder. LC-MS: tR=5.27; [M+H]+=467.04.

出典