HRID1833431

反应详情

EQUATION

反应方程式

HRID 1833431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

6-(2-phenylacetamido)-2,2-dimethyl-3-(O-methylphosphono)penam (384 mg., 1.0 millimole) is dissolved in 4 ml. of dry pyridine then trimethylchlorosilane (0.381 ml., 3.0 millimoles) and lithium iodide (536 mg., 4.0 millimoles) are added. The reaction mixture is stirred under nitrogen at 25° C. for 5 hours after which 2 ml. of water is added. The mixture is stirred for 10 minutes then the volatiles removed by evaporation in vacuo. The residue was taken up in water, adjusted to pH 8.0 and extracted with 3 × 10 ml. of chloroform. The aqueous phase was then acidified to pH 1.5 and extracted with 3 × 10 ml. of ethyl acetate. The ethyl acetate extracts were dried over sodium sulfate then evaporated to dryness to obtain the title compound.

WORKUP

后处理

  1. stirringThe mixture is stirred for 10 minutes
  2. customthe volatiles removed by evaporation in vacuo
  3. extractionextracted with 3 × 10 ml
  4. extractionextracted with 3 × 10 ml
  5. dry with materialThe ethyl acetate extracts were dried over sodium sulfate
  6. customthen evaporated to dryness