Dichloromethane → HCID 131719874, compound

Participants

Reaction Conditions

Reaction Steps

4-Chlorobutyryl chloride (12.69 g, 90 mmol) was mixed with paraldehyde (3.964 g, 30 mmol) and heated at 85° C. for 90 minutes. Additional paraldehyde (1.35 g) was added and the reaction mixture was stirred at 85° C. for an additional hour. The reaction mixture as cooled to room temperature, diluted with dichloromethane (100 ml) and stirred with saturated aqueous sodium bicarbonate (50 ml) at room temperature for 10 minutes. The dichloromethane layer was separated, dried over sodium sulfate and concentrated in vacuo to yield Cl(CH2)3CO2CHClCH3 which was vacuum distilled (55°-58° C. at 0.1 mm, 9.65 g, 58.6% yield) whose structure was confirmed by NMR.

Provenance & Evidence