4-Hydroxy-4-methylcyclohexanone → (4-Methoxy-4 methyl-cyclohexylidene)-acetic acid methyl ester

HRID 72854

反応式

HRID 72854 の反応式
[CH3:1][O:2][C:3]([CH2:5]P(OC)(OC)=O)=[O:4].[Li][CH2:13]CCC.[OH:17][C:18]1([CH3:25])[CH2:23][CH2:22][C:21](=O)[CH2:20][CH2:19]1>COCCOC>[CH3:1][O:2][C:3](=[O:4])[CH:5]=[C:21]1[CH2:22][CH2:23][C:18]([O:17][CH3:13])([CH3:25])[CH2:19][CH2:20]1

参加物

5

反応物 3

HCID 285394-Hydroxy-4-methylcyclohexanoneHCID 80029Trimethyl phosphonoacetateHCID 178418339Butyllithium

生成物 1

HCID 66742062(4-Methoxy-4 methyl-cyclohexylidene)-acetic acid methyl ester

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of trimethyl phosphonoacetate (9.11 mL, 56 mmol) and (40 mL, 64 mmol) of n-BuLi (1.6N) in DME (60 mL) is stirred for 10 minutes at 0° C. 4-Hydroxy-4-methyl-cyclohexanone (8 g, 56 mmol) was added and the mixture stirred 2.5 hours at 0° C. until TCL indicated complexion of the reaction. Product was obtained after extraction with dichloromethane (7.71 g, 69%).

後処理

  1. stirringthe mixture stirred 2.5 hours at 0° C. until TCL
  2. customcomplexion of the reaction
  3. customProduct was obtained
  4. extractionafter extraction with dichloromethane (7.71 g, 69%)

出典と根拠

ORDレコード
ord-d765b0a07c0e4665acc96698a2b2a4ee
出典データセット
uspto-grants-2014_09
特許番号
US08829029B2

関連ノート

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