Water → Cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid

HRID 370571

반응식

HRID 370571 반응식
[Cl:1][C:2](Cl)([Cl:12])[CH:3]1[CH:8]2[CH:6]([C:7]2([CH3:10])[CH3:9])[C:5](=[O:11])[O:4]1.O>C(O)(=O)C.CCOCC.[Zn]>[Cl:1][C:2]([Cl:12])=[CH:3][C@@H:8]1[C@H:6]([C:5]([OH:11])=[O:4])[C:7]1([CH3:9])[CH3:10]

참가 물질

6

반응물 2

HCID 962WaterHCID 125252184-Trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane

생성물 1

HCID 41507Cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid수율 97%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 176Acetic Acid용매HCID 3283Diethyl Ether용매3회

실험 절차

To a suspension of zinc powder (0.52 g, 0.008 mole) in 0.6 ml of acetic acid and 3 ml of ether was added dropwise over a period of 15 minutes a solution of 4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane (0.487 g, 0.002 mole) in 3 ml of ether. The mixture was stirred for two hours at room temperature, 30 ml of ether and 5 ml of water were added, and the mixture was then filtered through Celite filter aid. The organic layer was separated, washed twice with saturated aqueous sodium chloride, dried over magnesium sulfate, and the ether was evaporated to give crystalline cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylic acid (0.405 g, 97% yield).

후처리

  1. filtrationthe mixture was then filtered through Celite
  2. filtrationfilter aid
  3. customThe organic layer was separated
  4. washwashed twice with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. customthe ether was evaporated

출처 및 근거

ORD 기록
ord-b63ab4da8f0b40aa9d73b6f54d968290
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04526987

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