Hydrochloric Acid → 1-(5-Bromo-1,3-thiazol-2-yl)ethan-1-one

A solution of 5-bromo-2-(1,1-dimethoxyethyl)-1,3-thiazole (35 g) was dissolved in acetone (200 ml) and water (200 ml), was added con. HCl (40 ml). The mixture was stirred for 5 h at room temperature. After concentration to remove acetone, the residue was adjusted to pH=7 by the addition of NaHCO3 and extracted with ether (30 ml×3). The organic layers were washed with brine, dried over Na2SO4 and concentrated to afford 25 g of 1-(5-bromo-1,3-thiazol-2-yl)ethanone as solid (87.4%). 1H-NMR (CDCl3 400 MHz) δ 7.87 (s, 1H, Ar—H), 2.66 (s, 3H, —CH3)

1. concentrationAfter concentration
2. customto remove acetone
3. additionthe residue was adjusted to pH=7 by the addition of NaHCO3
4. extractionextracted with ether (30 ml×3)
5. washThe organic layers were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated

ORD record

ord-266e4b1777a9464ebbb59708489f5437

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08987310B2