Aluminium lithium hydride → 2-[(4-Chlorophenyl)methyl]azepane

HRID 27437

반응식

HRID 27437 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:22]=[CH:21][C:11]([CH2:12][CH:13]2[NH:19][C:18](=O)[CH2:17][CH2:16][CH2:15][CH2:14]2)=[CH:10][CH:9]=1>O1CCCC1>[Cl:7][C:8]1[CH:22]=[CH:21][C:11]([CH2:12][CH:13]2[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][NH:19]2)=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 233428517-(4-Chlorobenzyl)perhydroazepin-2-one

생성물 1

HCID 39338092-[(4-Chlorophenyl)methyl]azepane수율 68.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Add 0.5 g of lithium aluminum hydride to a solution of 2.8 g 7-(4-chlorobenzyl)-perhydroazepin -2-one in 30 ml of tetrahydrofurane. Boil the mixture under reflux for 16 hours, cool it and then carefully treat it with ice-water. After extraction with diethyl ether, dry the extract over sodium sulfate concentrate the oily residue and distill in a vacuum to obtain 1.8 g of the title compound with a BP of 90° to 92° at 0.05 mm Hg.

후처리

  1. temperatureBoil the mixture under reflux for 16 hours
  2. temperaturecool it
  3. extractionAfter extraction with diethyl ether
  4. customdry the
  5. extractionextract over sodium sulfate
  6. concentrationconcentrate the oily residue
  7. distillationdistill in a vacuum

출처 및 근거

ORD 기록
ord-32cc92d9280349b984ea48408cc67dba
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221788

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