تفاعل #8703

معادلة التفاعل

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

2-phenyl-ethanesulfonic acid amide potassium salt

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

المردود 90.3%

المذيبات

water

DMSO

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted twice with diethyl ether (75 ml) before it
2. 2
   استخلاصThe mixture was extracted twice with EA (150 ml)
3. 3
   غسيلThe organic phase was washed with water (50 ml)
4. 4
   أخرىThe product precipitated upon evaporation of the solvent
5. 5
   أخرىThe solid was collected
6. 6
   غسيلwashed with diethyl ether
7. 7
   أخرىdried

الإجراء التجريبي

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.

المصدر