反应详情

A stirred, ice water cooled mixture of 10.25 g (0.0302 mol) of 6,11-dihydro-N-(1-hydroxy-2-methyl-2-propyl)-11-oxodibenz[b,e]oxepin-2-yl acetamide of Example 2, and 100 ml of sieve dried CH2Cl2 was treated dropwise over a few minutes with 3.95 g (0.0332 mol) of thionyl chloride. The solution was then stirred 15 minutes with cooling and overnight (about 16 hours) at ambient temperature. The solution was washed with 10% sodium hydroxide solution, dried (Na2SO4) and concentrated to an oil which was dried by azeotropic distillation of toluene. On standing overnight at 5° C. the oil crystallized. Recrystallization from 12 ml of isopropanol afforded 6.10 g (62.9%) of crystals of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)methyl-4,4-dimethyloxazoline, m.p. 101°-103.5° C.

1. washThe solution was washed with 10% sodium hydroxide solution
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated to an oil which
4. dry with materialwas dried by azeotropic distillation of toluene
5. waitOn standing overnight at 5° C.
6. customthe oil crystallized
7. customRecrystallization from 12 ml of isopropanol