反应详情

温度

22.5 °C

To 582 mg of 7β-[2-(2-thienyl)acetamido]-3-hydroxymethyl-3-cephem-4-carboxylic acid and 174 mg of 5-mercapto-1-methyl-1H-tetrazole was added 12 ml of ethyl acetate to make a solution. To the solution were added in sequence 0.25 ml of trimethyl phosphite and 0.2 ml of ether solution of hydrogen chloride (5mol/l), and the mixture was stirred at 20 to 25° C. for 3hours. To the reaction solution was added 10 ml of water, whose pH was adjusted to 2 with 2N HCl, which was then allowed to form two layers. The aqueous layer was taken, to which was added 10 ml of ethyl acetate. The mixture was allowed to form two layers. The organic layers were combined and washed with 5 ml of aqueous saline, which was dried over anhydrous magnesium sulfate, which was then concentrated under reduced pressure. To the concentrate was added ether, then precipitating powdery product was collected by filtration, washed and dried to give 804 mg (yield: 89%) of 3-(1-methyl-1H-tetrazol-5-yl) thiomethyl-7β-[2-(2-thienyl)acetamido]-3-cephem-4-carboxylic acid.

1. customto form two layers
2. customto form two layers
3. washwashed with 5 ml of aqueous saline, which
4. dry with materialwas dried over anhydrous magnesium sulfate, which
5. concentrationwas then concentrated under reduced pressure
6. additionTo the concentrate was added ether
7. filtrationprecipitating powdery product was collected by filtration
8. washwashed
9. customdried