反応 #8703

反応方程式

4-[4,6-dichloro-5-(3-methoxy-phenoxy)-pyrimidin-2-yl]-morpholine

2-phenyl-ethanesulfonic acid amide potassium salt

→

2-phenyl-ethanesulfonic acid [6-chloro-5-(3-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidin-4-yl]-amide

収率 90.3%

溶媒

water

DMSO

反応条件

後処理

1. 1
   抽出extracted twice with diethyl ether (75 ml) before it
2. 2
   抽出The mixture was extracted twice with EA (150 ml)
3. 3
   洗浄The organic phase was washed with water (50 ml)
4. 4
   その他The product precipitated upon evaporation of the solvent
5. 5
   その他The solid was collected
6. 6
   洗浄washed with diethyl ether
7. 7
   その他dried

実験手順

A solution of 4-[4,6-dichloro-5-(3-methoxy-phenoxy)-pyrimidin-2-yl]-morpholine (1.0 g) and 2-phenyl-ethanesulfonic acid amide potassium salt (1.57 g, Referential Example 1e) in DMSO (15 ml) was stirred at 60° C. for 24 h. The solution was diluted with water (75 ml) and extracted twice with diethyl ether (75 ml) before it was acidified with 10% aq. citric acid. The mixture was extracted twice with EA (150 ml). The organic phase was washed with water (50 ml). The product precipitated upon evaporation of the solvent. The solid was collected, washed with diethyl ether and dried to give 2-phenyl-ethanesulfonic acid [6-chloro-5-(3-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidin-4-yl]-amide (1.28 g) as off-white powder. LC-MS: tR=5.34 min, [M+1]+=505.12, [M−1]−=502.97.

出典