HRID2102818

反应详情

EQUATION

反应方程式

HRID 2102818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-[6-6,7-Dimethoxyquinazolin-4-ylamino)benzothiazol-2-yl]benzamide was prepared by heating a mixture of N-(6-aminobenzothiazol-2-yl)benzamide (IM 2, 30 mg, 0.111 mmol) and 4-chloro-6,7-dimethoxyquinazoline (Fluorochem, 25 mg, 0.111 mmol) in ethylene glycol (0.7 mL) to 100° C. for 2 h. Brine (25 mL) and saturated sodium hydrogencarbonate solution (25 mL) were added and the product was extracted with chloroform (3×40 mL). After drying out Na2SO4, the solvent was removed and the residue was purified by pTLC (petroleum ether:dichloromethane:methanol=12:14:3) to yield a yellow solid (19 mg, 41 μmol, 37%). LC/ESI-MS: m/z 458 [M+H]+; m/z=456 [M−H]−; Rt=2.88 min.

WORKUP

后处理

  1. temperatureby heating
  2. extractionthe product was extracted with chloroform (3×40 mL)
  3. dry with materialAfter drying out Na2SO4
  4. customthe solvent was removed
  5. customthe residue was purified by pTLC (petroleum ether:dichloromethane:methanol=12:14:3)