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

HRID 27437

反応式

HRID 27437 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32cc92d9280349b984ea48408cc67dba
出典データセット
uspto-grants-1980_09
特許番号
US04221788

関連ノート

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