HRID1099591

反应详情

EQUATION

反应方程式

HRID 1099591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

150 mg (0.599 mmol) of 1-(4-chlorophenyl)-4,4,4-trifluorobutane-1,3-dione [Katsuyama et al., Synthesis, 1321-1324 (1997)] and 171 mg (1.20 mmol) of methyl 3-amino-4-methylpent-2-enoate [Holz et al., J. Org. Chem. 68., 1701-1707 (2003)] in 2 ml of acetonitrile were reacted at reflux temperature overnight. The volatile components were then removed on a rotary evaporator. The residue was purified by preparative HPLC (mobile phase: acetonitrile/water, gradient 10:90→90:10). This gave 34 mg (16% of theory) of the target compound.

WORKUP

后处理

  1. temperatureat reflux temperature overnight
  2. customThe volatile components were then removed on a rotary evaporator
  3. customThe residue was purified by preparative HPLC (mobile phase: acetonitrile/water, gradient 10:90→90:10)