反应详情

At room temperature, add 14.25 gm. (50 mmole) of methyl 10,11-dihydrodibenzo[b,f][1,4]-thiazepin-11-one-3-carboxylate to a stirred mixture of 10.425 gm. (50 mmole) of phosphorous pentachloride in 50 ml. of phosphorous oxychloride. Stir for 30 minutes, add an additional 1 gm. of phosphorous pentachloride and continue stirring for one hour. Partition the reaction mixture between a mixture of 400 ml. of methylene chloride, 350 gm. of ice and 150 ml. of water. Separate the aqueous layer and extract with 50 ml. of methylene chloride. Wash the combined organic extracts with a mixture of 100 gm. of ice and 100 ml. of water. Dry the methylene chloride solution over magnesium sulfate, charcoal and filter. Evaporate the solution, take-up in 50 ml. of dry toluene and again evaporate. Take up the residue in 25 ml. of acetonitrile, cool in an ice bath and separate the precipitate by filtration to obtain the title product. (m.p. 134°-135.5° C.)

1. additionAt room temperature, add 14.25 gm
2. additionadd an additional 1 gm
3. customPartition the reaction mixture
4. additionbetween a mixture of 400 ml
5. customSeparate the aqueous layer
6. extractionextract with 50 ml
7. washWash the combined organic extracts
8. additionwith a mixture of 100 gm
9. dry with materialDry the methylene chloride solution over magnesium sulfate, charcoal
10. filtrationfilter
11. customEvaporate the solution
12. customof dry toluene and again evaporate
13. temperatureof acetonitrile, cool in an ice bath
14. customseparate the precipitate
15. filtrationby filtration