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

HRID 638112ノート

反応式

HRID 638112 の反応式
[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

参加物

3

反応物 1

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

生成物 1

HCID 38013451-benzylazetidin-3-ol収率 27%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c8376f4df32d4c37b6c0706cbf65bb24
出典データセット
uspto-grants-1985_12
特許番号
US04560507

反応ノート

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