Hydrochloric Acid → HCID 69044855, compound

Iodine (catalytic amount) was added to a mixture of magnesium (1.97 g, 81 mmol) and anhydrous THF (30 ml) under a nitrogen atmosphere, and the mixture was stirred at room temperature for 30 minutes. Subsequently, a solution of 2-chloro-6-(1,3-dibromopropyl)phenyl acetate (28.5 g, 77 mmol) in anhydrous THF (90 ml) was added to the mixture at 80° C. over 45 minutes. After the mixture was stirred at 80° C. for 1 hour, the mixture was further stirred at room temperature for 2 hours. The reaction mixture was ice-cooled and 1M hydrochloric acid (80 ml) was added thereto. The mixture was extracted with ethyl acetate (2×100 ml). The organic layer was combined and successively washed with water and a saturated aqueous NaCl solution, followed by drying with anhydrous sodium sulfate. After the solid was removed by filtration, the filtrate was concentrated to obtain 16.3 g of 2-chloro-6-cyclopropylphenyl acetate as a brown oil.

1. stirringAfter the mixture was stirred at 80° C. for 1 hour
2. stirringthe mixture was further stirred at room temperature for 2 hours
3. temperaturecooled
4. extractionThe mixture was extracted with ethyl acetate (2×100 ml)
5. washsuccessively washed with water
6. dry with materialby drying with anhydrous sodium sulfate
7. customAfter the solid was removed by filtration
8. concentrationthe filtrate was concentrated

ORD record

ord-e5747317dcde4a239d25657603cbeaf8

Source dataset

uspto-grants-2009_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07629494B2