反应详情

温度

-23 °C

To a stirred solution of 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepine (2 g) in THF (25 mL) at -78° C. was added 1.6 M hexane solution of n-butyl lithium (5.4 mL). After 25 minutes, 3-chloromethyl-6-bromopyridine (1.79 g) in THF (5 mL) was added. After 30 minutes, the temperature was raised to -23° C. After 30 minutes, an excess saturated solution of NH4Cl was added and the mixture was extracted with ether. The organic extract was dried over MgSO4 and concentrated. The residue was chromatographed over silica gel using 10% ethyl acetate in hexane as eluant. Appropriate fractions were pooled to give the title compound (2.8 g) as a thick gum.

1. waitAfter 30 minutes
2. waitAfter 30 minutes
3. extractionthe mixture was extracted with ether
4. extractionThe organic extract
5. dry with materialwas dried over MgSO4
6. concentrationconcentrated
7. customThe residue was chromatographed over silica gel using 10% ethyl acetate in hexane as eluant