反应详情

Triethylamine (44.5g., 0.44 mole) is added to a slurry of 6-amino-2,2-dimethyl-3-cyanopenam hydrochloride (46.6g., 0.2 mole) in methylene chloride (1500 ml.) at room temperature and the resulting mixture stirred for 20 minutes. Triphenylmethyl chloride (66.9 g., 0.24 mole) is added in one portion to the mixture which is stirred at room temperature for 3.5 hours. The methylene chloride layer is separated and washed with water (5 × 100 ml.). It is then dried (Na2SO4) and concentrated in vacuo to orange-red viscous oil. Methanol (50 ml.) is added and the mixture stirred for a half hour to give a yellow-white solid. The solid is filtered, resuspended in fresh methanol, and the suspension stirred for a half hour. The solid is recovered by filtration and dried in a vacuum over at room temperature. Yield of crude = 47 gms. M.p. 116°-119° C.

1. stirringis stirred at room temperature for 3.5 hours
2. customThe methylene chloride layer is separated
3. washwashed with water (5 × 100 ml.)
4. dry with materialIt is then dried (Na2SO4)
5. concentrationconcentrated in vacuo to orange-red viscous oil
6. additionMethanol (50 ml.) is added
7. stirringthe mixture stirred for a half hour
8. customto give a yellow-white solid
9. filtrationThe solid is filtered
10. stirringthe suspension stirred for a half hour
11. filtrationThe solid is recovered by filtration
12. customdried in a vacuum over at room temperature