반응 #362924

반응 방정식

O-phenylhydroxylamine hydrochloride

4,4-piperidinediol hydrochloride

HCl

→

1,2,3,4-tetrahydrobenzo-furo[3,2-c]pyridine hydrochloride

수율 64.1%

용매

2-propanol

반응 조건

후처리

1. 1
   온도The reaction mixture was gently heated
2. 2
   온도to reflux temperature
3. 3
   workup.STIRRINGThe reaction mixture was stirred
4. 4
   온도refluxed for 3 hours
5. 5
   온도cooled to room temperature
6. 6
   여과The precipitate was filtered off
7. 7
   세척washed with diisopropyl ether
8. 8
   기타dried
9. 9
   기타This fraction was crystallized from water (1600 ml)
10. 10
    기타to crystallize out
11. 11
    workup.STIRRINGwhile stirring
12. 12
    여과The precipitate was filtered off
13. 13
    세척washed with 2-propanol and diisopropyl ether
14. 14
    기타dried

실험 절차

A mixture of O-phenylhydroxylamine hydrochloride (1:1) (0.625 mol) and 4,4-piperidinediol hydrochloride (1:1) (0.682 mol) in 2-propanol (615 ml) was stirred at 20° C. HCl (353 ml) was added dropwise at 20 ° C. The reaction mixture was gently heated to reflux temperature. The reaction mixture was stirred and refluxed for 3 hours, then cooled to room temperature. The precipitate was filtered off, washed with diisopropyl ether, and dried. This fraction was crystallized from water (1600 ml). The desired compound was allowed to crystallize out while stirring. The precipitate was filtered off, washed with 2-propanol and diisopropyl ether, then dried, yielding 84 g (64%) of 1,2,3,4-tetrahydrobenzo-furo[3,2-c]pyridine hydrochloride (1:1) (interm. 1).

출처