反应详情

温度

35 °C

Crude 4-acetoxy-2-methyl-1-chloro-2-butene (194 g, Purity: 83.8%, 1 mol) was added to hexamethylenetetramine (168 g, 1.2 mol)/water (1 liter), and the mixture was stirred at 35° C. for 4 hours and then separated into aqueous and organic layers. 1,2-Dichloroethane (1 liter) was added to the aqueous layer, the mixture was subjected to reaction at 72° C. for 6 hours while adjusting the pH with 1N sulfuric acid. The 1,2-dichloroethane layer was separated, 1,2-dichloroethane (1 liter) was added, and the reaction was carried out again. The 1,2-dichloroethane layers were combined and concentrated. The residue was distilled under reduced pressure to give 4-acetoxy-2-methyl-2-buten-1-al (98 g, 69%). bp.0.2-0.3 : 58°-66° C.

1. customseparated into aqueous and organic layers
2. addition1,2-Dichloroethane (1 liter) was added to the aqueous layer
3. customthe mixture was subjected to reaction at 72° C. for 6 hours
4. customThe 1,2-dichloroethane layer was separated
5. addition1,2-dichloroethane (1 liter) was added
6. concentrationconcentrated
7. distillationThe residue was distilled under reduced pressure