4-Chlorobutyryl chloride → 5-(4-Chlorobutyryl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one

HRID 36856

反応式

HRID 36856 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[CH:8]1[C:18]2[C:17](=[O:19])[NH:16][C:15]3[CH:20]=[CH:21][CH:22]=[CH:23][C:14]=3[NH:13][C:12]=2[CH:11]=[CH:10][CH:9]=1>CC(C)=O>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([N:13]1[C:12]2[CH:11]=[CH:10][CH:9]=[CH:8][C:18]=2[C:17](=[O:19])[NH:16][C:15]2[CH:20]=[CH:21][CH:22]=[CH:23][C:14]1=2)=[O:6]

参加物

4

反応物 2

HCID 783704-Chlorobutyryl chlorideHCID 2013275,10-Dihydro-11H-dibenzo(b,e)(1,4)diazepin-11-one

生成物 1

HCID 538563175-(4-Chlorobutyryl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 4-chlorobutyryl chloride (3.5 g) and 10,11-dihydrodibenzo[b,e][1,4]diazepin-11-one (4.2 g) (J. Med. Chem., 1963, 6, 767) in acetone (90 ml) was heated under reflux for 8 hours and evaporated. The residue was purified by chromatography on silica using hexane plus 0-100% dichloromethane as eluant. Appropriate fractions were combined and evaporated and the residue triturated with hexane/dichloromethane to give the title compound as a colourless solid, 1.62 g (26%), m.p. 151°-152° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 8 hours
  3. customevaporated
  4. customThe residue was purified by chromatography on silica
  5. customevaporated
  6. customthe residue triturated with hexane/dichloromethane

出典と根拠

ORDレコード
ord-79eaf72784de43c4af5c7a91e5d67ae8
出典データセット
uspto-grants-1995_05
特許番号
US05418229

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