反応 #10358

反応方程式

citric acid

N-ethyidiisopropylamine

benzylsulfamic acid amide potassium salt

4-[4,6-Dichloro-5-(2-methoxy-phenoxy)-pyrimidin-2-yl]-pyridine-2-carbonitrile

→

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

収率 93.0%

溶媒

DMSO

反応条件

後処理

1. 1
   workup.ADDITIONpoured onto ice/water
2. 2
   ろ過the precipitate was filtered off
3. 3
   その他recrystallized
4. 4
   その他form EtOAc

実験手順

4-[4,6-Dichloro-5-(2-methoxy-phenoxy)-pyrimidin-2-yl]-pyridine-2-carbonitrile (3.2 g) was dissolved in DMSO (20 ml), N-ethyidiisopropylamine (1.7 ml) and benzylsulfamic acid amide potassium salt (3.52 g) was added. The mixture was stirred for 18 h at rt, poured onto ice/water, acidified with solid citric acid and the precipitate was filtered off and recrystallized form EtOAc to give benzylsulfamic acid [6-chloro-2-(2-cyano-pyridin-4-yl)-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide (4.17 g). LC-MS: tR=5.55; [M+H]+=523.29.

出典