Diazomethane → 2-(4-Chlorobenzoyl)-2-(4-chlorophenyl)oxirane

HRID 231731

反応式

HRID 231731 の反応式
[N+](=C)=[N-].N(CN[C:8](N)=[O:9])=O.[OH-].[Na+].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([C:22]([C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=2)=O)=[O:21])=[CH:16][CH:15]=1>CCOCC.O1CCOCC1>[Cl:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]([C:22]2([C:24]3[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=3)[CH2:8][O:9]2)=[O:21])=[CH:18][CH:19]=1

参加物

7

反応物 4

HCID 9550DiazomethaneHCID 14798Sodium HydroxideHCID 189461,2-Ethanedione, 1,2-bis(4-chlorophenyl)-HCID 104823Urea, (nitrosomethyl)-

生成物 1

HCID 198700842-(4-Chlorobenzoyl)-2-(4-chlorophenyl)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 by reaction of 5.34 g of N-nitrosomethylurea with aqueous sodium hydroxide solution in ether is added dropwise to a solution of 5 g of 4,4'-dichlorobenzil in 50 ml of dioxane. When the dropwise addition is complete, stirring is continued for 16 hours at room temperature, and the reaction solution is then concentrated by evaporation. The residual oil is crude 2-(4-chlorobenzoyl)-2-(4-chlorophenyl)oxirane which is purified by high vacuum distillation.

後処理

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

出典と根拠

ORDレコード
ord-6d4cb271441e4f7d8ae60d44ed921d4b
出典データセット
uspto-grants-1989_07
特許番号
US04849007

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