2,3-Dichloro-5-(chloromethyl)pyridine → 2,3-Dichloro-5-(methoxymethyl)pyridine

温度

60 °C

Under argon and at room temperature, 4.14 g (23 mmol) of sodium methoxide (30 percent strength solution in methanol) was added dropwise within 5 minutes to a solution of 4.11 g (20.9 mmol) of 2,3-dichloro-5-(chloromethyl)-pyridine [prepared from 2,3-dichloro-5-(hydroxymethyl)-pyridine by reaction with thionyl chloride] in 40 ml of methanol. The reaction mixture was subsequently heated to 60° C. for 3 hours. After the reaction had ended, the solvent was distilled off and the residue was admixed with 100 ml of water and extracted with dichloromethane (3×75 ml). The organic phase was dried over magnesium sulfate and evaporated. The yield of the product was 4.06 g (90.4 percent) of a yellow oil, purity (GC) 90.8 percent.

1. distillationthe solvent was distilled off
2. extractionextracted with dichloromethane (3×75 ml)
3. dry with materialThe organic phase was dried over magnesium sulfate
4. customevaporated

ORDレコード

ord-417f070d4f034bef938334c2140ee6ab

出典データセット

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05925765