反应详情

Add 6.34 gm. (20 mmole) of finely powdered methyl 10,11-dihydro-11-oxodibenzo[b,f][1,4]thiazepin-3-carboxylate 5,5-dioxide to a mixture of 6.25 gm. (30 mmole) phosphorous pentachloride in 17.3 ml. of phosphoryl chloride. Stir for 18 hours at room temperature. Separate the solids by filtration, wash with ether and dry in vacuo over potassium hydroxide. Dissolve the crude product in boiling tetrahydrofuran, filter and evaporate to a small volume in a stream of nitrogen. Dilute with acetonitrile and separate the precipitate by filtration in order to obtain the title product. (m.p. 254°-256° C.).

1. additionAdd 6.34 gm
2. customSeparate the solids
3. filtrationby filtration
4. washwash with ether
5. dry with materialdry in vacuo over potassium hydroxide
6. dissolutionDissolve the crude product
7. filtrationfilter
8. customevaporate to a small volume in a stream of nitrogen
9. additionDilute with acetonitrile
10. customseparate the precipitate
11. filtrationby filtration in order