반응 #40361

반응 방정식

4-(2-chloro-pyrimidin-4-yloxy)-2,5-dimethyl-phenylamine

N-methylaniline

ethyl acetate

→

[4-(4-Amino-2,5-dimethyl-phenoxy)-pyrimidin-2-yl]-methyl-phenyl-amine

용매

hydrochloric acid

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타the organic layer was separated
3. 3
   여과the formed precipitate was filtered by suction
4. 4
   세척washed with hexane
5. 5
   기타After separation the organic layer
6. 6
   농축was concentrated in vacuo and column chromatography (dichloromethane)
7. 7
   기타yielded 380 mg (11%) with a purity of 89% log P (pH=2.3)=1.72

실험 절차

A solution of 2.50 g (10 mmol) 4-(2-chloro-pyrimidin-4-yloxy)-2,5-dimethyl-phenylamine and 2.14 g N-methylaniline (20 mmol) in 50 ml hydrochloric acid were stirred for 20 h at 80° C. After cooling down to ambient temperature 50 ml ethyl acetate was added and the organic layer was separated. The water layer was brought to pH 8 with sodium carbonate and the formed precipitate was filtered by suction and washed with hexane. After separation the organic layer was concentrated in vacuo and column chromatography (dichloromethane) yielded 380 mg (11%) with a purity of 89% log P (pH=2.3)=1.72.

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