HRID1038710
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of (6-chloro-pyrimidin-4-yl)-ethyl-amine (363 mg, 2.30 mmol, 1.1 eq.) and 4-(4-methylpiperazin-1-yl)-aniline (400 mg, 2.09 mmol) in water (0.8 ml) and glacial acetic acid (3.2 ml) is heated to 100° C. 3 h. After solvent evaporation, the residue is taken up in methanol, made alkaline by addition of 25% NH3 in water and concentrated. The residue is purified by MPLC (silica gel) (DCM/MeOH) to afford 395 mg of the title compound as a white solid: ESI-MS: 313.2 [MH]+; tR=1.25 min (purity: ˜90%, gradient J); TLC: Rf=0.12 (DCM/MeOH, 9:1).
WORKUP
后处理
- custom3 h
- customAfter solvent evaporation
- additionby addition of 25% NH3 in water
- concentrationconcentrated
- customThe residue is purified by MPLC (silica gel) (DCM/MeOH)