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

HRID 231730

반응식

HRID 231730 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-068a47997e2c45ea9953c3a15c70f647
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04849007

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