HRID241411

反应详情

EQUATION

反应方程式

HRID 241411 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3 ml of 4M HCl in dioxane are added to tert-butyl 4-[6′-amino-5′-(6-methoxy-1 H-benzimidazol-2-yl)-[3,3′]bipyridinyl-6-yl]piperazine-1-carboxylate, and the mixture is stirred at room temperature for 14 h. The reaction mixture is evaporated to dryness, and water is added. The aqueous phase is adjusted to pH>10 using 2N NaOH and extracted 3× with ethyl acetate. The organic phases are dried using sodium sulfate, filtered and evaporated. The residue is purified by means of RP-HPLC and lyophilised, giving 5-(6-methoxy-1H-benzimidazol-2-yl)-6′-piperazin-1-yl-[3,3′]bipyridinyl-6-ylamine as free base; HPLC-MS [M+H]+ 402.2.

WORKUP

后处理

  1. customThe reaction mixture is evaporated to dryness, and water
  2. additionis added
  3. extractionextracted 3× with ethyl acetate
  4. customThe organic phases are dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by means of RP-HPLC