Trimethyl 2-chloro-2-cyclopropylidenorthoacetate: Cyclopropane,

Trimethyl 2-chloro-2-cyclopropylidenorthoacetate Cyclopropane, (1 -chloro-2,2,2-trimethoxyethylidene)- (11) (82979-34-8)... 

A. Trimethyl 2-chloro-2-cyclopropylidenorthoacetate. A 1-L, two-necked, round-bottomed flask equipped with a mechanical stirrer and a reflux condenser is charged with 40.0 g (0.19 mol) of 1-chloro-1-(trichloroethenyl)cyclopropane (Note 1), 120 g of potassium hydroxide, and 300 mLof methanol (Note 2). The mixture is stirred for 16-18 hr in an oil bath at 85°C. After the solution is cooled to room temperature, it is diluted with 1 L of ice water. The mixture is then transferred to a 3-L separatory funnel and extracted with three 200-mL portions of ether. The combined ether phases are washed with three 150-mL portions of saturated brine, dried over anhydrous magnesium sulfate, and filtered. The solvent is removed from the filtrate by distillation at atmospheric pressure, and the residue is distilled through a short-path column under water-aspirator vacuum to give 14.5-15.4 g (39-41%) of trimethyl 2-chloro-2-cyclopropylidenorthoacetate, bp lOS-IOS C (20 mm) (Notes 3 and 4). 

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See also in sourсe #XX -- [ , , ]

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