2,6-Dichloro-4-methylpyridine → HCID 84116020, compound

Participants

Reaction Steps

In a sealed vial, a solution of 2,6-dichloro-4-picoline (1.80 g, 11.1 mmol) in diethylamine (5 mL) is heated to 135° C. for 40 h in a microwave oven. The pressure in the vial reaches 6.5 bar. The mixture is diluted with EA (200 mL) and washed with 1 N KHSO4, solution. The washings are extracted back with EA (100 mL) and the combined org. extracts are dried over MgSO4, filtered and concentrated. The crude product is purified by CC on silica gel eluting with heptane:EA 95:5 to give (6-chloro-4-methyl-pyridin-2-yl)-diethyl-amine (1.15 g) as a colourless solid; LC-MS: tR=1.05 min, [M+1]+=198.97.

Provenance & Evidence