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

HRID 1379314

反応式

HRID 1379314 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 26250Potassium ferricyanide触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-105c3e5c5b0e4119ac2b972ffb7869fe
出典データセット
uspto-grants-1997_09
特許番号
US05670692

関連ノート

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