Water → 4-(4-Chlorophenyl)-alpha-(4-fluorophenyl)-4-hydroxy-1-piperidinebutanol

HRID 1578388

반응식

HRID 1578388 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[CH:33]=[CH:32][C:11]([C:12]([CH2:14][CH2:15][C:16]([N:18]2[CH2:23][CH2:22][C:21]([C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=3)([OH:24])[CH2:20][CH2:19]2)=O)=[O:13])=[CH:10][CH:9]=1.O>O1CCCC1>[F:7][C:8]1[CH:9]=[CH:10][C:11]([CH:12]([OH:13])[CH2:14][CH2:15][CH2:16][N:18]2[CH2:19][CH2:20][C:21]([C:25]3[CH:26]=[CH:27][C:28]([Cl:31])=[CH:29][CH:30]=3)([OH:24])[CH2:22][CH2:23]2)=[CH:32][CH:33]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 215599881-(4-(4-Chlorophenyl)-4-hydroxypiperidin-1-yl)-4-(4-fluorophenyl)butane-1,4-dione

생성물 1

HCID 1192654-(4-Chlorophenyl)-alpha-(4-fluorophenyl)-4-hydroxy-1-piperidinebutanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of 2.0 g of lithium aluminum hydride and 50 ml of tetrahydrofuran, was gradually added a solution of 5.0 g of 1-[β-(p-fluorobenzoyl)propionyl]-4-(p-chlorophenyl)-4-hydroxypiperidine in 40 ml of tetrahydrofuran. The mixture was stirred at room temperature for one hour, and at 60°to 65°C for 4 hours. Then 15 ml of cold water was added dropwise to the reaction mixture while the mixture was kept below 20°C in an ice bath. The precipitate was filtered off and the tetrahydrofuran was removed from the filtrate by distillation under reduced pressure. The residue was kept cooled for 2 hours and the solid matter was collected by filtration, washed with water, and dried to obtain 1-(p-fluorophenyl)-4-[4-(p-chlorophenyl)-4-hydroxypiperidino]-1 -butanol, melting at 128° - 130°C.

후처리

  1. waitat 60°to 65°C for 4 hours
  2. customwas kept below 20°C in an ice bath
  3. filtrationThe precipitate was filtered off
  4. customthe tetrahydrofuran was removed from the filtrate by distillation under reduced pressure
  5. temperatureThe residue was kept cooled for 2 hours
  6. filtrationthe solid matter was collected by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-4eb8283397294fecad7c0920a9cb540b
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03936468

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