HRID2049562

反应详情

EQUATION

反应方程式

HRID 2049562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Aminocephalosporanic acid (5.44 g., 20 mmole) and 5-Mercapto-1H-tetrazol-1-ylacetamide (3.50 g., 2.2 mmole) were suspended in 50% aqueous acetone (200 ml) and solid sodium bicarbonate added until a clear solution was obtained, ~pH 7.0. The solution was heated at 60° for 6 hours, uncovered for the final hour which allowed most of the acetone to evaporate, then acidified to pH 4.0 and stirred in an ice bath for one hour. The solid product was collected, washed with a little cold water and dried in vacuo, 3.22 g (43.4%), δ(CF3CO2H) 4.00 (2H,bs, C2 methylene), 4.69 (2H,bs, --CH2S--), 5.56 (4H,s, --CH2CO2NH2 and β-lactam protons), 7.4-7.8 (2H,m, --CONH2).

WORKUP

后处理

  1. customwas obtained
  2. temperatureThe solution was heated at 60° for 6 hours
  3. customto evaporate
  4. customThe solid product was collected
  5. washwashed with a little cold water
  6. dry with materialdried in vacuo, 3.22 g (43.4%), δ(CF3CO2H) 4.00 (2H,bs, C2 methylene), 4.69 (2H,bs, --CH2S--), 5.56 (4H,s, --CH2CO2NH2 and β-lactam protons), 7.4-7.8 (2H,m, --CONH2)