HRID446651

反应详情

EQUATION

反应方程式

HRID 446651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19 ml of a 4M solution of HCl in dioxane are added to 2.3 g of 4-(2-(4-(tert-butoxycarbonyl)piperazin-1-yl)ethoxy)-2,6-bis(hydroxymethyl)pyridine in solution in 33 ml of dioxane. After 12 h at AT, the resulting precipitate is recovered by filtration on a sintered glass funnel, taken up in MeOH and then concentrated under RP, and the residue is diluted in 40 ml of an MeOH/water 1/1 mixture. The resulting solution is deposited on Mega BE-SCX, 25GM 150ML (Varian). After washing the phase with MeOH, the product of interest is eluted with a 2N solution of ammonia in methanol. The MeOH/NH3 phase is concentrated under RP. 1.6 g of 4-[2-(piperazin-1-yl)ethoxy]-2,6-bis(hydroxymethyl)pyridine are thus obtained.

WORKUP

后处理

  1. filtrationthe resulting precipitate is recovered by filtration on a sintered glass funnel
  2. concentrationconcentrated under RP
  3. additionthe residue is diluted in 40 ml of an MeOH/water 1/1 mixture
  4. washAfter washing the phase with MeOH
  5. washthe product of interest is eluted with a 2N solution of ammonia in methanol
  6. concentrationThe MeOH/NH3 phase is concentrated under RP