反应详情

温度

0 °C

2.58 g of 2,3,4,5-tetrahydro-8-nitro-2-oxo-1H-1-benzazepine dissolved in 30 ml of abs. dimethylformamide were added to 650 mg of 55% NaH in 20 ml of abs. dimethylformamide. The mixture was stirred for 1 hour, then cooled to 0° C. and 1.35 ml of methyl iodide were slowly added dropwise thereto. After 45 minutes the mixture was poured on ice, extracted with ethyl acetate, washed with NaCl solution, dried and evaporated. Flash chromatography on silica gel (hexane/ethyl acetate=1/1) yielded 2.46 g of 2,3,4,5-tetrahydro-1-methyl-8-nitro-2-oxo-1H-1-benzazepine as orange crystals of m.p. 151°-152° C.

1. additionAfter 45 minutes the mixture was poured on ice
2. extractionextracted with ethyl acetate
3. washwashed with NaCl solution
4. customdried
5. customevaporated