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

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Reaction Steps

130 g of the above-obtained oil containing N-methoxy-2,4-dibromobutyric acid amide were dissolved in 500 mL of benzene. To the resultant solution, 12 g of sodium hydride were gradually added while cooling the solution to 15° C. to 20° C. After the completion of the addition, ice was added to the resultant reaction solution to decompose excessive sodium hydride. The resultant solution was washed with a saturated saline, followed by drying the solution by magnesium sulfate. The solution was concentrated under a reduced pressure and purified by silica gel-acetone/benzene column chromatography. Consequently, 39 g (0.2 mol) of N-methoxy-2-bromo-4-butyrolactam (with a yield of 36% from 2,4-dibromobutyric acid bromide) was obtained.

Provenance & Evidence