1,2-Dichloroethane → 2-Methyl-4-(1-oxopropoxy)-2-butenal

温度

35 °C

The crude 4-propionyloxy-2-methyl-1-chloro-2-butene (64.0 g, 0.362 mol) obtained in the above (i) was added to a solution of hexamethylenetetramine (50.9 g, 0.363 mol) in water (345 ml), and the mixture was stirred at 35° C. for 4 hours to prepare a tetramine salt. 1,2-Dichloroethane (200 ml) was added to the reaction mixture, and compounds insoluble in water were removed by extraction. 1,2-Dichloroethane (400 ml) was further added to the aqueous layer that had been washed, and the mixture was stirred at 60° C. for 4 hours to hydrolyze the tetramine salt. After completion of the reaction, the 1,2-dichloroethane layer was separated, and 1,2-dichloroethane (250 ml) was further added to the aqueous layer for extraction. The 1,2-dichloroethane layers were combined and dried over anhydrous sodium sulfate. The 1,2-dichloroethane was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate-hexane (=1:5)) to give 4-propionyloxy-2-methyl-2-buten-1-al (15.2 g, 0.0973 mol, Yield: 26.8% ).

1. customwere removed by extraction
2. addition1,2-Dichloroethane (400 ml) was further added to the aqueous layer that
3. washhad been washed
4. stirringthe mixture was stirred at 60° C. for 4 hours
5. customAfter completion of the reaction
6. customthe 1,2-dichloroethane layer was separated
7. addition1,2-dichloroethane (250 ml) was further added to the aqueous layer for extraction
8. dry with materialdried over anhydrous sodium sulfate
9. customThe 1,2-dichloroethane was evaporated under reduced pressure
10. customthe residue was purified by silica gel column chromatography (ethyl acetate-hexane (=1:5))

ORDレコード

ord-058f1754f95a4ac2af5d634a51172185

出典データセット

uspto-grants-1995_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05424478