Hydrochloric Acid → Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester
Reaktionsgleichung
[Na].Cl.[CH3:3][C:4]([CH3:17])([CH:11](Cl)[CH:12]=[C:13]([Cl:15])[Cl:14])[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7]>C(O)C>[CH3:3][C:4]1([CH3:17])[CH:11]([CH:12]=[C:13]([Cl:15])[Cl:14])[CH:5]1[C:6]([O:8][CH2:9][CH3:10])=[O:7]Komponenten
Versuchsvorschrift
Thereafter, 2.8 parts of metallic sodium were dissolved in 150 parts of anhydrous ethanol, and 27.4 parts of ethyl 3,3-dimethyl-4,6,6-trichloro-5-hexenoate prepared by the process described above, were added to the solution. The mixture was agitated for 2 hours under reflux of ethanol. The reaction mixture was cooled by ice water and neutralized with hydrogen chloride-saturated ethanol solution. The precipitated solids were removed by filtration, and ethanol was distilled from the filtrate. The filtrate was diluted with diethyl ether, washed with water and then dried on anhydrous magnesium sulfate. The solvent was removed by distillation, and the residue was subjected to distillation under reduced pressure to obtain 21.0 parts of ethyl 2,2-dimethyl-3-(2',2'-dichlorovinyl)cyclopropane carboxylate having a boiling point of 72° to 73° C. under 0.3 mmHg. The yield was 89%. The cis:trans ratio of the product determined by gas chromatography was 25:75.
Aufarbeitung
- customprepared by the process
- additionwere added to the solution
- customThe precipitated solids were removed by filtration, and ethanol
- distillationwas distilled from the filtrate
- additionThe filtrate was diluted with diethyl ether
- washwashed with water
- dry with materialdried on anhydrous magnesium sulfate
- customThe solvent was removed by distillation
- distillationthe residue was subjected to distillation under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-fb6bb0f4dd47400ebd5e30816935ef27
- Quelldatensatz
- uspto-grants-1980_02
- Patentnummer
- US04190730
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