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

HRID 1080918

反応式

HRID 1080918 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+].[K+].[Fe+6]>[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 11963580Ferrate(4-), hexakis(cyano-C)-, tetrapotassium, (OC-6-11)-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 (IlI) 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-427b5ac39657440192b4dbdfe0242632
出典データセット
uspto-grants-1996_12
特許番号
US05583247

関連ノート

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