반응 #5257
ord-80f62c1c46ba4eb9a6ba6a91577ca2ab
반응 방정식
반응물
시약
반응 조건
후처리
- 1기타were reacted
- 2기타to obtain 27.1 g of raw product
- 3기타precipitation
- 4여과filtered
- 5세척the product was rinsed with acetic acid, acetone
- 6기타ether to obtain 4.6 of product
- 7여과vacuum filtered
- 8세척The product was rinsed with water, acetone
실험 절차
Using the procedure of Step A of Example 8, 27.2 g of 7-amino-cephalosporanic acid, 128 ml of the etherate of boron trifluoride, 126 ml of benzyl alcohol and 90 ml of triethylamine were reacted to obtain 27.1 g of raw product. 25 g of the said product and 250 ml of acetic acid were added to 25 ml of the etherate of boron trifluoride followed by the addition of 25 ml of triethylamine which caused precipitation. The mixture was vacuum filtered and the product was rinsed with acetic acid, acetone and then ether to obtain 4.6 of product. 4.8 g of the said product were dissolved at 45° C. in 20 ml of 2N hydrochloric acid and 8 ml of concentrated hydrochloric acid and the solution was treated with activated carbon. 6 ml of ammonium hydroxide were added to the mixture which was then vacuum filtered. The product was rinsed with water, acetone and then ether to obtain 2 g of 3-benzyloxy-7-amino-ceph-3-eme-4-carboxylic acid.