反应详情

温度

75 °C

Sodium hydride (60% dispersion in mineral oil, 1.28 g, 45 mmol) was suspended in DMF (20 mL) and cooled in an ice bath under a nitrogen atmosphere. (2-Chloro-phenyl)-acetonitrile (1.77 g, 11.7 mmol) in DMF (5 mL) was added slowly, and the mixture stirred for 2 hours. Bis-(2-chloro-ethyl)-carbamic acid tert-butyl ester (3.3 g, 11.1 mmol) in DMF (5 mL) was then added and the mixture heated to 75° C. for 6 hours. The solvent was removed by evaporation under vacuum and the residue dissolved in ethyl acetate (50 mL), washed with water, then brine, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum. The residue was purified by silica chromatography eluting with a mixture of ethyl acetate and hexane. The fractions containing the desired products were combined and the solvent removed by evaporation to give the title compound as an orange gum (1.1 g). LCMS m/z 321.0 [M+H]+. R.T.=4.76 min (Analytical Method 4).

1. temperaturecooled in an ice bath under a nitrogen atmosphere
2. customThe solvent was removed by evaporation under vacuum
3. dissolutionthe residue dissolved in ethyl acetate (50 mL)
4. washwashed with water
5. dry with materialbrine, dried over magnesium sulphate
6. filtrationfiltered
7. customthe solvent removed by evaporation under vacuum
8. customThe residue was purified by silica chromatography
9. washeluting with a mixture of ethyl acetate and hexane
10. additionThe fractions containing the desired products
11. customthe solvent removed by evaporation