HRID324163
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 30 °C
PROCEDURE
实验过程
To a solution of biotinamido-N-methyl-glycine methyl ester in methanol is added 1.5-2.0 equivalents of 1 N aqueous sodium hydroxide. The mixture is stirred at 15-45° C. for 4-24 h and then concentrated via reduced pressure rotary evaporation. The residue is diluted with deionized water and the pH of the solution is adjusted to 1-2 by addition of 6 N aqueous hydrochloric acid. The mixture is again concentrated via reduced pressure rotary evaporation. The residue is chromatographed on reverse phase C-18 silica gel, and eluted with methanol/water. The fractions containing the product are combined and concentrated to afford the final product (5).
WORKUP
后处理
- concentrationconcentrated via reduced pressure rotary evaporation
- additionThe residue is diluted with deionized water
- additionthe pH of the solution is adjusted to 1-2 by addition of 6 N aqueous hydrochloric acid
- concentrationThe mixture is again concentrated via reduced pressure rotary evaporation
- customThe residue is chromatographed on reverse phase C-18 silica gel
- washeluted with methanol/water
- additionThe fractions containing the product
- concentrationconcentrated