HRID993316

反应详情

EQUATION

反应方程式

HRID 993316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 2-(4-fluorophenyl)-3-(4-(methylthio)phenyl)-3-oxopropanoate(1.33 g, 4 mmol), prepared according to the method of Example 1A(ii), hydrazine hydrate (0.25 mL, 4.2 mmol), and acetic acid (0.25 mL, 4.2 mmol) in dioxane (50 mL), and water (5 mL) was refluxed for 24 hours and then concentrated in vacuo. Water was added to the residue, and the solid was filtered and dried in vacuo to provide the desired product (yield: 1.15 g; 95%). MS (DCI-NH3) m/z 301 (M+H)+, 318 (M+NH4)+; 1H NMR (300 MHz, DMSO-d6) δ2.47 (s, 3H), 7.12 (t, J=9 Hz, 2H), 7.26 (m, 6H).

WORKUP

后处理

  1. customprepared
  2. temperaturewas refluxed for 24 hours
  3. concentrationconcentrated in vacuo
  4. additionWater was added to the residue
  5. filtrationthe solid was filtered
  6. customdried in vacuo