HRID1110452

反应详情

EQUATION

反应方程式

HRID 1110452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-aminoethyl dihydrogen phosphate (56 mg, 0.4 mmol) in water (0.35 ml) and triethylamine (0.3 ml, 2 mmol) was added to mitomycin A (referred to hereinafter as "MMA") (140 mg, 0.4 mmol) in methanol (6 ml) and the reaction was allowed to proceed at room temperature overnight. 1.4 ml of saturated aqueous sodium bicarbonate was then added and the solution was partitioned between water and methylene chloride. The aqueous phase was concentrated to dryness and several portions of methanol were added and evaporated. The residue was taken up into methanol, filtered, and applied to a 2×10 cm C-18 (reverse phase) silica column. The product was eluted with water and all volatile material was evaporated. Methanol was added and evaporated as before and the residue was dried for 24 h under high vacuum in a desiccator with phosphorus pentoxide. The mitomycin phosphate derivative, MOP, was obtained as a fine blue powder (190 mg, 97%).

WORKUP

后处理

  1. customthe solution was partitioned between water and methylene chloride
  2. concentrationThe aqueous phase was concentrated to dryness and several portions of methanol
  3. additionwere added
  4. customevaporated
  5. filtrationfiltered
  6. washThe product was eluted with water
  7. customall volatile material was evaporated
  8. additionMethanol was added
  9. customevaporated as before and the residue
  10. dry with materialwas dried for 24 h under high vacuum in a desiccator with phosphorus pentoxide