Sodium hydride → 3-Bromo-1-methoxypyrrolidin-2-one

1400 g of a crude N-methoxy-2,4-dibromobutanamide was dissolved in 5 liters of benzene. Then 125 g of NaH was added little by little to the solution at 15° to 20° C. while the reaction mixture was cooled with an iced water bath. After the reaction, the remaining NaH was decomposed with ice and the product mixture was washed with a saturated, aqueous salt solution. It was dried with magnesium sulfate. Then benzene was distilled out. The product was purified with the column chromatography, using silica gel and a mixture of acetaone and benzene to obtain 500 g of the title compound 4.

1. temperaturewas cooled with an iced water bath
2. customAfter the reaction
3. washthe product mixture was washed with a saturated, aqueous salt solution
4. dry with materialIt was dried with magnesium sulfate
5. distillationThen benzene was distilled out
6. customThe product was purified with the column chromatography
7. additiona mixture of acetaone and benzene

ORD record

ord-836c58a4370e47af9d9e01d3b6d301fa

Source dataset

uspto-grants-1989_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04833160