反应详情

Sodium nitrite (1.84 g, 26.7 mmol) was dissolved in 32 ml of concentrated sulfuric acid at 0° C. Then, 6-(4-benzyloxyphenoxy)pyridin-3-ylamine (7.1 g, 24.29 mmol) in 75 ml of acetic acid were slowly added dropwise. After 1 h the ice bath was removed and stirring was continued for an hour. The reaction mixture was added dropwise to 250 ml of boiling water, and the mixture was stirred for 1 hour and after cooling extracted with ethyl acetate. The precipitated solid was filtered off and the filtrate was concentrated and purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 269 mg (4%), M+H+: 294.10.

1. customAfter 1 h the ice bath was removed
2. waitwas continued for an hour
3. additionThe reaction mixture was added dropwise to 250 ml of boiling water
4. stirringthe mixture was stirred for 1 hour
5. temperatureafter cooling
6. extractionextracted with ethyl acetate
7. filtrationThe precipitated solid was filtered off
8. concentrationthe filtrate was concentrated
9. custompurified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)