HRID1056358

反应详情

EQUATION

反应方程式

HRID 1056358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A glass microwave reaction vessel was charged with N1,N1-bis(2-methoxyethyl)-3-methylbutane-1,3-diamine (50 mg, 0.229 mmol) and 8-iodo-3-methyl-2-(methylsulfinyl)quinazolin-4(3H)-one (700b; 80 mg, 0.229 mmol) in tBuOH (0.5 mL). The reaction mixture was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc.) at 120° C. for 45 min. Similarly another two batches (50 mg and 170 mg) were carried out. The three batches were combined and the solvent was removed. The residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM) to give 2((4-(bis(2-methoxyethyl)amino)-2-methylbutan-2-yl)amino)-8-iodo-3-methylquinazolin-4(3H)-one (210 mg, 0.42 mmol). MS (ESI, pos. ion) m/z: 503 (M+1).

WORKUP

后处理

  1. customA glass microwave reaction vessel
  2. customthe solvent was removed
  3. customThe residue was purified with silica gel chromatography (eluted with 0-5% MeOH in DCM)