반응 #1742422

반응 방정식

K2CO3

trifluoroacetic anhydride

4,5-dichloro-2-methyl-pyridine-N-oxide

methanol

→

4,5-dichloro-2-hydroxy- methylpyridine

용매

H2O

dichloromethane

반응 조건

후처리

1. 1
   온도The solution was cooled to 5°-10°
2. 2
   추출extracted with chloroform
3. 3
   건조The extract was dried (K2CO3)
4. 4
   기타the residue triturated with petrol

실험 절차

To a stirred and cooled solution of 4,5-dichloro-2-methyl-pyridine-N-oxide (8.54 g) in dichloromethane (110 ml) at 10°-15°, was added trifluoroacetic anhydride (12 ml) and the reaction mixture allowed to stand 6 days. The solution was cooled to 5°-10°, methanol added dropwise and the mixture stripped. The residue was treated with H2O (70 ml) basified to pH 9-10 (K2CO3) and extracted with chloroform. The extract was dried (K2CO3), stripped and the residue triturated with petrol to give 4,5-dichloro-2-hydroxy- methylpyridine, (6.15 g), m.p. 103°-106°

출처