Ketene dimethyl acetal → Ethyl (3,3-dimethoxycyclobutylidene)acetate

HRID 1476125노트

반응식

HRID 1476125 반응식
[CH3:1][O:2][C:3]([O:5][CH3:6])=[CH2:4].[C:7]([O:12][CH2:13][CH3:14])(=[O:11])[CH:8]=[C:9]=[CH2:10]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1([O:5][CH3:6])[CH2:10][C:9](=[CH:8][C:7]([O:12][CH2:13][CH3:14])=[O:11])[CH2:4]1

참가 물질

4

반응물 2

HCID 136706Ketene dimethyl acetalHCID 4066088Ethyl 2,3-butadienoate

생성물 1

HCID 58288413Ethyl (3,3-dimethoxycyclobutylidene)acetate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 3.93 g (44.59 mmol) of 1,1-dimethoxyethene and 5 g (44.59 mmol) of ethyl buta-2,3-dienoate in 50 ml of toluene was heated at reflux and stirred for 24 h. After cooling to room temperature, the reaction mixture was freed from the solvent, and the crude product obtained was purified chromatographically on silica gel (mobile phase cyclohexane/ethyl acetate 20:1). This gave 1.9 g (21% of theory) of the title compound as a colourless liquid which was used without further characterization for subsequent reactions.

후처리

  1. temperatureat reflux

출처 및 근거

ORD 기록
ord-f7cb47885d63462faa1e80b80783e245
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018414B2

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