HRID870674

反应详情

EQUATION

反应方程式

HRID 870674 反应方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A stirred mixture of (3-amino-propyl)-methyl-carbamic acid isopropyl ester (3.0 g, 17.0 mmol), 3-bromo-6-chloro-imidazo[1,2-b]pyridazine [13526-66-4] (723.7 mg, 3.1 mmol), and Hunig's base [7087-68-5] (0.6 mL, 3.2 mmol) was heated to 85° C., under N2 blanket, for 3d then preabsorbed on silica gel and flash chromatographed (silica gel eluted with 10% (v/v) methanol/ethyl acetate) to obtain 1.0 g of clear yellow oil. LRMS (ESI) m/z 370.2/372.2 [(M+H)]+, calc'd for C14H20BrN5O2: 370.25.

WORKUP

后处理

  1. customfor 3d then preabsorbed on silica gel and flash
  2. customchromatographed
  3. wash(silica gel eluted with 10% (v/v) methanol/ethyl acetate)