1-Chloro-4-(chloromethyl)benzene → HCID 22923790, compound

Participants

Reaction Steps

8.4 g (60 mmol) of 3-hydroxypyridine-2-carboxylic acid were alkylated (3 h, 110° C.) with 5.2 g (approximately 130 mmol, 60%) of sodium hydride and 19.3 g (120 mmol) of 4-chlorobenzyl chloride in N,N-dlmethylacetamide in analogy with Example 30a). After concentration in vacuo and extraction with Na bicarbonate solution, the residue was purified on silica gel using heptane/ethyl acetate (1:1), and 14.8 g of the product were crystallized from appropriate fractions using diisopropyl ether, m.p. 92°-94° C.

Provenance & Evidence