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3-Chloropropionyl chloride → 3-Chloro-1-(4-formyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1-propanone

HRID 429729
ノート
印刷プレビュー

反応式

HRID 429729 の反応式
[CH:1]([N:3]1[CH2:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[O:6][CH2:5][CH2:4]1)=[O:2].[Cl:14][CH2:15][CH2:16][C:17](Cl)=[O:18].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[Cl:14][CH2:15][CH2:16][C:17]([C:11]1[CH:12]=[CH:13][C:7]2[O:6][CH2:5][CH2:4][N:3]([CH:1]=[O:2])[CH2:9][C:8]=2[CH:10]=1)=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 693643-Chloropropionyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 118195761,4-Benzoxazepine-4(5H)-carboxaldehyde, 2,3-dihydro-

生成物 1

HCID 183526783-Chloro-1-(4-formyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1-propanone収率 75.9%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

To a solution of 1.7 g of 4-formyl-2,3,4,5-tetrahydro-1,4-benzoxazepine and 1.28 g of 3-chloropropionyl chloride in 20 ml of 1,2-dichloroethane was added 3.0 g of aluminum chloride by portions. The mixture was stirred for 6 hours under reflux. The reaction mixture was poured into ice-water, and the resultant was subjected to extraction with dichloromethane. The extract was washed with water, dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (developing solvent: ethyl acetate) to give 1.95 g of the title compound as a colorless oily substance.

後処理

  1. temperatureunder reflux
  2. extractionthe resultant was subjected to extraction with dichloromethane
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by means of silica gel column chromatography (developing solvent: ethyl acetate)

出典と根拠

ORDレコード
ord-048863db7e434cf49fc24558ed2b8f71
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06319916B1

反応ノート

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