3-Bromo-1-propanol → 3-Bromopropyl 3-oxobutanoate

90 g of 3-bromopropanol was added to 8 g of sodium acetate, to which 59.8 g of diketene was added dropwise controlling the reaction mixture at 40°-50° C. The mixture was further stirred at room temperature for 3 hours. The reaciton mixture was poured into ice water containing a diluted aqueous sodium hydroxide solution. The mixture was extracted with dichloromethane and the dichloromethane layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain 102.6 g of 3-bromopropyl acetoacetate.

1. additionwas added dropwise
2. customat 40°-50° C
3. extractionThe mixture was extracted with dichloromethane
4. washthe dichloromethane layer was washed with a saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off

ORD record

ord-562c52ec74c042609d0828ddbd368e14

Source dataset

uspto-grants-1984_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04472411