Bromochloromethane → HCID 22236954, compound

A solution of 20 g of the compound obtained in Step 1 in 400 ml of THF was stirred at −78° C. under atmosphere of nitrogen, and then, 45 ml of 2M lithium diisopropylamide solution was slowly added thereto. The resulting mixture was stirred for one hour and thereto was slowly added a solution of 13.62 g of bromochloromethane in 30 ml of THF. After one hour, the resulting mixture was stirred at room temperature for four hours. After the reaction was completed, an aqueous ammonium chloride solution was added, the reaction mixture was extracted with ethyl acetate. The organic phase was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and the residue thus obtained was purified by a silica gel column chromatography using a mixture of ethyl acetate and n-hexane of 1:6 to obtain 19.14 g of the title compound as an oil.

1. waitAfter one hour
2. stirringthe resulting mixture was stirred at room temperature for four hours
3. extractionthe reaction mixture was extracted with ethyl acetate
4. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customthe residue thus obtained
7. customwas purified by a silica gel column chromatography
8. additiona mixture of ethyl acetate and n-hexane of 1:6

ORD record

ord-a46adac91750492daf48648a0f582394

Source dataset

uspto-grants-2006_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07012144B2