Potassium Hydroxide → N,N-Diethyl-2-(3,5-di-tert-butyl-4-oxocyclohexa-2,5-dienylidene)acetamide

HRID 1379314

반응식

HRID 1379314 반응식
[CH2:1]([N:3]([CH2:22][CH3:23])[C:4](=[O:21])[CH2:5][C:6]1[CH:11]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:9]([OH:16])=[C:8]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:7]=1)[CH3:2].[OH-].[K+]>ClCCl.O.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[K+].[K+].[K+].[Fe+3]>[CH2:22]([N:3]([CH2:1][CH3:2])[C:4](=[O:21])[CH:5]=[C:6]1[CH:11]=[C:10]([C:12]([CH3:14])([CH3:15])[CH3:13])[C:9](=[O:16])[C:8]([C:17]([CH3:20])([CH3:19])[CH3:18])=[CH:7]1)[CH3:23]

참가 물질

6

반응물 2

HCID 14797Potassium HydroxideHCID 18924148N,N-Diethyl-2-(3,5-di-tert-butyl-4-hydroxyphenyl)acetamide

생성물 1

HCID 22019858N,N-Diethyl-2-(3,5-di-tert-butyl-4-oxocyclohexa-2,5-dienylidene)acetamide수율 75.6%

시약·촉매·용매 3

HCID 26250Potassium ferricyanide촉매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

4.80 g (0.015 Mol) of N,N-diethyl- 2-(3,5-di-tert-butyl-4-hydroxy-phenyl)acetamide are dissolved in 60 ml of dichloromethane. To this solution a solution of 15 g (0.046 mol) of potassium hexacyanoferrate (III) and 6.0 g (0.11 mol) of potassium hydroxide in 120 ml of water is added, and the mixture is stirred one hour at room temperature under nitrogen. The organic layer is separated, washed with water and evaporated in vacuo. The solid residue is recrystallized from acetonitrile to give 3.6 g of the title compound as yellow needles, melting at 109°-110° C.

후처리

  1. customThe organic layer is separated
  2. washwashed with water
  3. customevaporated in vacuo
  4. customThe solid residue is recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-105c3e5c5b0e4119ac2b972ffb7869fe
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05670692

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