反应详情

温度

35 °C

A mixture of 0.11 mole of nitronium tetrafluoroborate and 60 g. tetramethylene sulfone is stirred at 10° C. and 0.1 mole of 3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-2'-oxirane, prepared as described in Example 57, Step A, added during 30 minutes. The cooling bath then is removed and the mixture stirred an additional 20 minutes at 35° C., poured into ice and water, the product extracted with ether, the ether solution dried over magnesium sulfate and evaporated. The product obtained following crystallization from a mixture of chloroform and petroleum ether is 7-nitro-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-2'-oxirane.

1. additionadded during 30 minutes
2. customThe cooling bath then is removed
3. additionpoured into ice and water
4. extractionthe product extracted with ether
5. dry with materialthe ether solution dried over magnesium sulfate
6. customevaporated
7. customThe product obtained
8. customcrystallization
9. additionfrom a mixture of chloroform and petroleum ether