反应详情

To a stirred and ice-cooled solution of 1-azido-4-methoxy-benzene (1.000 g, 6.7046 mmol) and 2,4-difluoro phenyl acetonitrile (1.27 g, 8.0455 mmol) in absolute ethanol (20 ml), an ice-cooled solution of sodium methoxide (0.543 g, 10.0569 mmol) in absolute ethanol (10 ml) is added drop-wise. The resulting reaction mixture is evaporated and the residue is dissolved in methylene chloride and washed with water, brine, dried over MgSO4, filtered and evaporated to afford ˜2 g of crude material as brownish solid. This material is purified by crystallization from methylene chloride and petroleum ether, to obtain the title compound as brown solid (1.10 g, 48% yield). M.p. 152-156.5° C. LC-ESI-HRMS of [M+H]+ shows 303.1046 Da. Calc. 303.105742 Da, dev. −3.8 ppm.

1. additionis added drop-wise
2. customThe resulting reaction mixture
3. customis evaporated
4. dissolutionthe residue is dissolved in methylene chloride
5. washwashed with water, brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated
9. customto afford ˜2 g of crude material as brownish solid
10. customThis material is purified by crystallization from methylene chloride and petroleum ether