反应详情

温度

0 °C

A suspension of sodium hydride (0.06 g) in N,N-dimethylformamide (3 ml) is cooled to 0° C. 7-fluoro-3,4-dihydro-3-oxo-6-nitro-2H-1,4-benzoxazine (0.57 g) is added thereto at between 0° to 5° C., and the resultant mixture is stirred for 30 minutes. Propargyl bromide (0.35 g) is added to the mixture, which is gradually heated to room temperature, and the reaction is continued for 6 hours. After addition of water, the resultant mixture is extracted with ethyl acetate, and the extract is washed with water, dried and concentrated. The residue is purified by silica gel thin layer chromatography using a 1:1 mixture of ethyl acetate and n-hexane as the eluent to give 7-fluoro-3,4-dihydro-3-oxo-6-nitro-4-(2-propynyl)-2H-1,4-benzoxazine.

1. temperatureis gradually heated to room temperature
2. extractionthe resultant mixture is extracted with ethyl acetate
3. washthe extract is washed with water
4. customdried
5. concentrationconcentrated
6. customThe residue is purified by silica gel thin layer chromatography
7. additiona 1:1 mixture of ethyl acetate and n-hexane as the eluent