Diazomethane → 2-(2,4-Dichlorobenzoyl)-2-(2,4-dichlorophenyl)oxirane

HRID 231730

反応式

HRID 231730 の反応式
[N+](=C)=[N-].N(CN[C:8](N)=[O:9])=O.[OH-].[Na+].[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1[C:21]([C:23]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][C:26]=1[Cl:32])=O)=[O:22]>CCOCC.O1CCOCC1>[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1[C:21]([C:23]1([C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][C:26]=2[Cl:32])[CH2:8][O:9]1)=[O:22]

参加物

7

反応物 4

HCID 9550DiazomethaneHCID 14798Sodium HydroxideHCID 104823Urea, (nitrosomethyl)-HCID 133916831,2-Bis(2,4-dichlorophenyl)ethane-1,2-dione

生成物 1

HCID 198700832-(2,4-Dichlorobenzoyl)-2-(2,4-dichlorophenyl)oxirane

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

実験手順

With cooling and stirring, an ethereal diazomethane solution prepared from 3.1 g of nitrosomethylurea and aqueous sodium hydroxide solution in ether is added dropwise to a solution of 3.4 g of 2,2',4,4'-tetrachlorobenzil in 50 ml of dioxane. When the dropwise addition is complete, stirring is continued for 16 hours at room temperature, and the reaction mixture is then concentrated to dryness. The residual oil is crude 2-(2,4-dichlorobenzoyl)-2-(2,4-dichlorophenyl)oxirane which is purified by high vacuum distillation.

後処理

  1. temperatureWith cooling
  2. additionWhen the dropwise addition
  3. stirringstirring
  4. concentrationthe reaction mixture is then concentrated to dryness
  5. distillationis purified by high vacuum distillation

出典と根拠

ORDレコード
ord-068a47997e2c45ea9953c3a15c70f647
出典データセット
uspto-grants-1989_07
特許番号
US04849007

関連ノート

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