Hydrochloric Acid → HCID 69479868, compound

(S)-2-Chloro-4-nitro-1-[2-hydroxy-3-(4-nitrobenzoyloxy)-2-methylpropyl]imidazole prepared in Example 15 (6.8 g, 17.67 mmol) was dissolved in methanol (68 ml). Potassium carbonate (122 mg, 0.88 mmol) was added to the solution, and the resulting mixture was stirred at room temperature overnight. The mixture was cooled on ice-bath, 6N hydrochloric acid (0.3 ml) and magnesium sulfate (3 g) were added to the mixture in this order, and the mixture was stirred for 30 minutes. Insoluble matters were removed by filtration, and the filtrate was concentrated under reduced pressure. Ethyl acetate (3.4 ml) and toluene (34 ml) were added to the residue, and the resulting precipitates were filtered off to afford (S)-2-chloro-1-(2,3-dihydroxy-2-methylpropyl)-4-nitroimidazole (4.09 g, yield 97%) as a yellow powder.

1. temperatureThe mixture was cooled on ice-bath
2. stirringthe mixture was stirred for 30 minutes
3. customInsoluble matters were removed by filtration
4. concentrationthe filtrate was concentrated under reduced pressure
5. additionEthyl acetate (3.4 ml) and toluene (34 ml) were added to the residue
6. customthe resulting precipitates
7. filtrationwere filtered off

ORD record

ord-770b5bd5350e41968cbd00c66484b1fc

Source dataset

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07262212B2