Benzyl-(1-amino-3-chloro-2-propanol) → 1-benzylazetidin-3-ol

HRID 638112노트

반응식

HRID 638112 반응식
[CH2:1]([NH:8][CH2:9][CH:10]([OH:13])[CH2:11]Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>O>[CH2:1]([N:8]1[CH2:11][CH:10]([OH:13])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

3

반응물 1

HCID 173441Benzyl-(1-amino-3-chloro-2-propanol)

생성물 1

HCID 38013451-benzylazetidin-3-ol수율 27%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

10 g of 1A was heated under reflux in 150 ml of water with stirring for 24 hours. The reaction mixture was cooled, the aqueous solution was decanted from insoluble material and made alkaline by the addition of solid sodium hydroxide. The oil which separated was extracted with dichloromethane and the extracts were washed with water and dried. The solvent was removed under reduced pressure and the residue was purified by chromatography on silica gel using acetone as eluent, followed by recrystallization from toluene to give 1, as a crystalline solid, m.p.: 64.5°-65.5° C., in 27% yield.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customthe aqueous solution was decanted from insoluble material
  3. additionby the addition of solid sodium hydroxide
  4. customThe oil which separated
  5. extractionwas extracted with dichloromethane
  6. washthe extracts were washed with water
  7. customdried
  8. customThe solvent was removed under reduced pressure
  9. customthe residue was purified by chromatography on silica gel
  10. customfollowed by recrystallization from toluene
  11. customto give 1

출처 및 근거

ORD 기록
ord-c8376f4df32d4c37b6c0706cbf65bb24
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04560507

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