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

HRID 72854

반응식

HRID 72854 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
0 °C

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-d765b0a07c0e4665acc96698a2b2a4ee
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829029B2

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