Water → 2,2-Dimethyl-3-methylthiocyclopropane-1-carboxylic acid methyl ester

HRID 1680801

반응식

HRID 1680801 반응식
[CH3:1][O:2][C:3]([C:5]1(C(OC)=O)[CH:7]([CH3:8])[C:6]1([CH3:10])[CH3:9])=[S:4].O.[Br-].[Na+]>O=P1(C)CCC=C1>[CH3:1][O:2][C:3]([CH:5]1[CH:7]([CH3:8])[C:6]1([CH3:10])[CH3:9])=[S:4]

참가 물질

5

반응물 3

HCID 962Water2회HCID 253881Sodium BromideHCID 887684162,2-Dimethyl-3-methylthio-cyclopropane-1,1-dicarboxylic acid dimethyl ester

생성물 1

HCID 887707122,2-Dimethyl-3-methylthiocyclopropane-1-carboxylic acid methyl ester수율 75.8%

시약·촉매·용매 1

HCID 701042,3-Dihydro-1-methyl-1H-phosphole 1-oxide용매

실험 절차

23 g (0.1 mol) of 2,2-dimethyl-3-methylthio-cyclopropane-1,1-dicarboxylic acid dimethyl ester (prepared according to J. Chem. Soc., Chem. Comm. 1972 (7), 375) were dissolved in 25 ml of 1-oxo-1-methylphospholine and 2 ml of water and the solution was heated to 180° C. with 8 g of sodium bromide for 12 hours. The mixture was then cooled, poured into water, extracted by shaking with toluene and distilled. 12 g (=69% of theory) of 2,2-dimethyl-3-methylthiocyclopropane-1-carboxylic acid methyl ester of boiling point 75° C./3 mm Hg are obtained.

후처리

  1. temperatureThe mixture was then cooled
  2. extractionextracted
  3. distillationdistilled

출처 및 근거

ORD 기록
ord-6e4dea2e83f2409fa9d9c2d84f8eb01f
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276225

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