Pyridine → HCID 14093552、化合物

反応式

[CH3:1][C:2]([CH2:9][CH3:10])([CH2:7]O)[C:3]([O:5][CH3:6])=[O:4].S(Cl)([Cl:13])=O.N1C=CC=CC=1>>[CH3:1][C:2]([CH2:9][CH3:10])([CH2:7][Cl:13])[C:3]([O:5][CH3:6])=[O:4]

参加物

反応物 3

HCID 1049Pyridine

HCID 24386Thionyl Chloride2 回

HCID 14093550116623-21-3

生成物 1

HCID 14093552HCID 14093552、化合物収率 93.2%

反応条件

温度: 50 °C

実験手順

The methyl 2-methyl-2-ethyl-3-hydroxypropionate was added at below 20° C. to 178.6 g (1.5 mol) of thionyl chloride, and the mixture was stirred at 50° C. for a further 30 min. Excess thionyl chloride was then distilled off at 100 mbar, 0.5 g (0.006 mol) of pyridine was added to the residue, and the mixture was heated at from 130° to 135° C. for 45 min. Fractional distillation gave 114.4 g of methyl 2-methyl-2-ethyl-3-chloropropionate having a boiling point of 101°-104° C./8 mbar, corresponding to a 93.2% yield, based on methyl 2-methyl-2-ethyl-3-hydroxypropionate. The overall yield was 69.5%, based on 2-methyl-2-ethyl-3-hydroxypropanal.