تفاعل #8704

معادلة التفاعل

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

ethylene glycol

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

المذيبات

citric acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was cooled to rt
2. 2
   استخلاصextracted twice with EA (150 ml)
3. 3
   غسيلThe organic phase was washed with water (50 ml)
4. 4
   أخرىevaporated
5. 5
   أخرىThe crude product was purified by chromatography on silica gel eluting with heptane:EA 1:1 to 1:2

الإجراء التجريبي

A suspension of 2-phenyl-ethanesulfonic acid [6-chloro-5-(3-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidin-4-yl]-amide (1.27 g) in ethylene glycol (12 ml) was treated with K-tert.-butylate (2.82 g). The resulting solution was stirred at 100° C. for 12 d. The solution was cooled to rt, diluted with 10% aq. citric acid (150 ml) and extracted twice with EA (150 ml). The organic phase was washed with water (50 ml) and evaporated. The crude product was purified by chromatography on silica gel eluting with heptane:EA 1:1 to 1:2 to furnish 2phenyl-ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidin-4-yl]-amide (1.1 g) as a white solid. LC-MS: tR=4.66 min, [M+1]+=531.20, [M−1]−=529.14.

المصدر