反应详情

Sodium hydride (3.36 g of a 50% dispersion in mineral oil) was added portionwise to a stirred solution of the product of part (i) (17.43 g) in dry tetrahydrofuran (200 ml) and the mixture was stirred at room temperature for 1 hour. 4-Fluoronitrobenzene (9.87 g) was added dropwise and the mixture was stirred for a further 18 hours and then evaporated. Water was added to the residue and the mixture was extracted several times with dichloromethane. The combined extracts were washed with water, dried (MgSO4) and evaporated to give an oil which solidified on trituration with ether. The solid was filtered off, washed with a little ether and crystallised from ethyl acetate/hexane to give the product, (13.51 g), m.p. 121°-122°.

1. stirringthe mixture was stirred for a further 18 hours
2. customevaporated
3. additionWater was added to the residue
4. extractionthe mixture was extracted several times with dichloromethane
5. washThe combined extracts were washed with water
6. dry with materialdried (MgSO4)
7. customevaporated
8. customto give an oil which
9. filtrationThe solid was filtered off
10. washwashed with a little ether
11. customcrystallised from ethyl acetate/hexane
12. customto give the product, (13.51 g), m.p. 121°-122°