Sodium Chloride → Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester

HRID 1680800

반응식

HRID 1680800 반응식
[CH2:1]([O:3][C:4]([C:6]1(C(OCC)=O)[CH:8]([CH:9]=[C:10]([Cl:12])[Cl:11])[C:7]1([CH3:14])[CH3:13])=[O:5])[CH3:2].O=P1(C)CCC=C1.[Cl-].[Na+]>O>[CH2:1]([O:3][C:4]([CH:6]1[CH:8]([CH:9]=[C:10]([Cl:11])[Cl:12])[C:7]1([CH3:13])[CH3:14])=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 5234Sodium ChlorideHCID 701042,3-Dihydro-1-methyl-1H-phosphole 1-oxideHCID 14914133Ethyl 2-(2,2-dichlorovinyl)-3,3-dimethyl-1-ethoxycarbonylcyclopropanecarboxylate

생성물 1

HCID 101094Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester수율 90%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

30 g (0.1 mol) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1,1-dicarboxylic acid diethyl ester, 50 ml of 1-oxo-1-methyl-phospholine, 6 g of sodium chloride and 4 ml of water were heated to 175° C. for 9 hours. The mixture was then cooled, poured into 150 ml of water and extracted with petroleum ether. After drying with MgSO4, the mixture was fractionally distilled. 21.3 g (=90% of theory) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-1-carboxylic acid ethyl ester of boiling point 65°-75° C./0.1 mm Hg were obtained. 49.7 g of 1-oxo-1-methyl-phospholine of boiling point 75°-77° C./0.15 mm Hg were recovered by fractional distillation of the aqueous phase.

후처리

  1. temperatureThe mixture was then cooled
  2. extractionextracted with petroleum ether
  3. dry with materialAfter drying with MgSO4
  4. distillationthe mixture was fractionally distilled

출처 및 근거

ORD 기록
ord-fc7aa8eebf7d4aa594b72af9cf0a8909
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276225

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