Hexane → 2-Chloro-5-(chloromethyl)pyridine

In 50 ml of water was suspended 15.0 g (0.07 mole) of 6-chloro-3-pyridylmethyl chloride hydrochloride and the suspension was adjusted to pH about 8 with a saturated aqueous solution of sodium hydrogen carbonate. The resulting mixture was extracted with ether (100 ml×3) and dried over MgSO4. The ether was then distilled off under reduced pressure to give a crystalline residue. After addition of hexane, the crystals were recovered by filtration, washed with hexane and dried to give 11.0 g of 6-chloro-3-pyridylmethyl chloride as white prisms.

1. extractionThe resulting mixture was extracted with ether (100 ml×3)
2. dry with materialdried over MgSO4
3. distillationThe ether was then distilled off under reduced pressure
4. customto give a crystalline residue
5. filtrationthe crystals were recovered by filtration
6. washwashed with hexane
7. customdried

ORD record

ord-6eb0a0317ca244b1862644549790a245

Source dataset

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05935981