HRID446646

反应详情

EQUATION

反应方程式

HRID 446646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 198 mg of tris(2-carboxyethyl)phosphine hydrochloride in 730 μl of water is added to 80 mg of 4-{2-[methyl(2-methyl-2-(methyldisulphanyl)propyl)amino]ethoxy}-2,6-bis(hydroxymethyl)pyridine in solution in 1.95 ml of methanol. After 2 h at AT, the mixture is concentrated under RP and the residue is taken up in 10 ml of water. The aqueous phase is brought to pH=8 by addition of an aqueous sodium hydroxide solution and then extracted 2× with AcOEt. The combined organic phases are washed with a saturated aqueous NaCl solution and concentrated under RP. 68 mg of 4-{2-[(2-mercapto-2-methylpropyl)(methyl)amino]ethoxy}-2,6-bis(hydroxymethyl)pyridine are obtained.

WORKUP

后处理

  1. concentrationthe mixture is concentrated under RP
  2. additionThe aqueous phase is brought to pH=8 by addition of an aqueous sodium hydroxide solution
  3. extractionextracted 2× with AcOEt
  4. washThe combined organic phases are washed with a saturated aqueous NaCl solution
  5. concentrationconcentrated under RP