反应详情

A mixture of 9.9 g of 2-tritylamino-4-thiazolylacetic acid, 100 ml of tetrahydrofuran and 2.7 ml of N-methylmorpholine was stirred under an inert gas for 15 minutes at room temperature and was then cooled to -15° C after which 3.15 ml of isobutyl chloroformate were added. The mixture was stirred for 5 minutes at -10° to -15° C and then 6.5 g of the product of Step A, 65 ml of water and 3.15 ml of triethylamine were added over 2 minutes. The mixture was stirred for 11/2 hours at room temperature and the tetrahydrofuran was removed. The mixture was acidified and was extracted with methylene chloride. The mixture was vacuum filtered and the organic phase was washed and evaporated to dryness. The powdery residue was triturated with ether and dried to obtain 15.2 g of raw product. 6.7 g of of the said product were dissolved in methylene chloride and ethyl acetate was added thereto. The insoluble phase was removed and the solution was treated with carbon black and was vacuum filtered. The recovered product was rinsed and dried to obtain 5.1 g of 7-[2-(2-tritylamino-4-thiazolyl)-acetamido]-3-acetylthiomethyl-ceph-3-eme-4-carboxylic acid.

1. additionwere added
2. stirringThe mixture was stirred for 5 minutes at -10° to -15° C
3. stirringThe mixture was stirred for 11/2 hours at room temperature
4. customthe tetrahydrofuran was removed
5. extractionwas extracted with methylene chloride
6. filtrationfiltered
7. washthe organic phase was washed
8. customevaporated to dryness
9. customThe powdery residue was triturated with ether
10. customdried
11. customto obtain 15.2 g of raw product
12. customThe insoluble phase was removed
13. additionthe solution was treated with carbon black
14. filtrationfiltered
15. washThe recovered product was rinsed
16. customdried