反应详情

温度

5 °C

In 60 ml of N,N-dimethylformamide were dissolved 20 g of trimethylsilylmethanol. This was maintained at 5° C. in a water bath and 4.6 g of sodium hydride were added thereto in the atmosphere of argon. The resulting mixture was stirred at 5° C. for 1 hour. Thereafter, 33.3 g of 3-nitrophthalonitrile dissolved in 160 ml of N,N-dimethylformamide were added dropwise to the mixture. After completion of the addition, the ice bath was removed and the mixture was stirred at room temperature for 24 hours. The reaction product was then added with 200 ml of dilute hydrochloric acid and extracted with 1 liter of toluene. The organic layer was washed well with water, followed by the removal of water with magnesium sulfate and the purification with a toluene/silica gel column. However, the desired compound shown by the above formula (XV) was hardly obtained. The yield was about 1% and 3-methoxyphthalonitrile as a by-product was yielded in an amount of several times that of the compound (XV).

1. additionwere added dropwise to the mixture
2. additionAfter completion of the addition
3. customthe ice bath was removed
4. stirringthe mixture was stirred at room temperature for 24 hours
5. additionThe reaction product was then added with 200 ml of dilute hydrochloric acid
6. extractionextracted with 1 liter of toluene
7. washThe organic layer was washed well with water
8. customfollowed by the removal of water with magnesium sulfate
9. customthe purification with a toluene/silica gel column
10. customwas hardly obtained