反应详情

温度

70 °C

N-methyl formanilide 19.4 ml (158 mmole), was chilled to 13° C., where it began to solidify. Phosphorus oxychloride, 13.7 ml (147 mmole), was added with stirring, under nitrogen. After 25 minutes, the temperature was 45° C. and the reaction had again begun to solidify. The compound of Step A, 14 g (95 mmole), was added and the mixture was stirred and heated in a 70° C. oil bath. The reaction exothermed to 95° C. Stirring was continued under nitrogen for 30 minutes. The bath was removed and when the temperature reached 350, the mixture was dissolved in chloroform. Ice was added and the layers were separated and washed once with water, twice with saturated sodium bicarbonate, once again with water and once with brine. The organic layer was chromatographed on 450 ml silica, eluting with chloroform to give 13.54 g (81%) of subtitled product which was used without further purification.

1. customwas 45° C.
2. stirringthe mixture was stirred
3. customexothermed to 95° C
4. stirringStirring
5. waitwas continued under nitrogen for 30 minutes
6. customThe bath was removed
7. dissolutionthe mixture was dissolved in chloroform
8. additionIce was added
9. customthe layers were separated
10. washwashed once with water, twice with saturated sodium bicarbonate, once again with water and once with brine
11. customThe organic layer was chromatographed on 450 ml silica
12. washeluting with chloroform