反应详情

To a solution of 4.2 g. of diphenylmethyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate in 44 ml. of dry dimethylformamide was added 865 mg. of phosphorus trichloride. The mixture was stirred for 1.5 hours at room temperature and was poured into an ethyl acetate 5% aqueous hydrochloric acid mixture. The ethyl acetate layer was evaporated, was washed with 5% hydrochloric acid, water and was dried. The dried solution was concentrated in vacuo and the product crystallized. The 3-chloro ester was filtered, washed with cold ethyl acetate and dried to yield 2.2 g.

1. customThe ethyl acetate layer was evaporated
2. washwas washed with 5% hydrochloric acid, water
3. customwas dried
4. concentrationThe dried solution was concentrated in vacuo
5. customthe product crystallized
6. filtrationThe 3-chloro ester was filtered
7. washwashed with cold ethyl acetate
8. customdried
9. customto yield 2.2 g