反应 #5083

反应方程式

Acetic anhydride

Virginiamycin M1

→

monoacetate

diacetate

溶剂

pyridine

反应条件

后处理

1. 1
   其他followed by flash evaporation to dryness at room temperature
2. 2
   其他The residue was partitioned between dichloromethane (3×300 ml) and saturated NaCl (aq, 300 ml)
3. 3
   干燥dried over anhydrous Na2SO4, flash
4. 4
   其他evaporated to dryness (dry weight=8.1 g)
5. 5
   其他purified over E

实验过程

Acetic anhydride (45 ml) was added to a stirring solution of Virginiamycin M1 (6.5 g) in anhydrous pyridine (45 ml) at room temperature. After 30 minutes, ice-cold methanol (85 ml) was added in portions. Stirring was continued for 20 more minutes followed by flash evaporation to dryness at room temperature. The residue was partitioned between dichloromethane (3×300 ml) and saturated NaCl (aq, 300 ml). The organic layers were pooled, dried over anhydrous Na2SO4, flash evaporated to dryness (dry weight=8.1 g) and purified over E. Merck silica gel 60 column in hexane/acetone mixtures to give 1.0 g of the monoacetate and 1.58 g of the diacetate.

来源