HRID1893727

反应详情

EQUATION

反应方程式

HRID 1893727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Aqueous hydrochloric acid (0.99 g of 37%) is added to a solution of 4-[(4-methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]-benzamide (4.94 g, 10 mmol) in ethanol (20 mL). The solution is evaporated to dryness under reduced pressure and the resulting residue is re-crystallized from ethanol-ethylacetate. The product is filtered-off and re-crystallized from isopropanol to afford, after filtering and drying, 4-[(4-methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]-benzamide, hydrochloride as a pale-yellow crystalline solid, having the following analytical properties: Analysis found: C, 65.27; H, 6.07; N, 18.19; Cl, 6.55%; H2O, 0.56%. Calculated for C29H32N7OCl-0.17 H2O: C, 65.33; H, 6.11; N, 18.39; Cl, 6.65%; H2O, 0.57%.

WORKUP

后处理

  1. customThe solution is evaporated to dryness under reduced pressure
  2. customthe resulting residue is re-crystallized from ethanol-ethylacetate
  3. customre-crystallized from isopropanol
  4. customto afford
  5. filtrationafter filtering
  6. customdrying