HRID1453877

反应详情

EQUATION

反应方程式

HRID 1453877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of dimethyl 4-benzyloxy-1-(2-nitrophenyl)-1H-pyrazole-3,5-dicarboxylate (2.0 g, 4.85 mmol) in MeOH (100 mL) was added palladium on carbon (200 mg). The mixture was then stirred and purged with hydrogen gas. The mixture was stirred at ambient temperature under 1 atmosphere of hydrogen gas for 72 hours. The mixture was filtered through celite and the filter cake was washed with MeOH. The filtrate solvent was removed under reduced pressure. Trituration of the residue in a small volume of MeOH gave the product as a white solid. 1H NMR (400 MHz, d6-DMSO) δ 11.65 (s, 1H), 9.74 (s, 1H), 8.07 (d, J=8.2 Hz, 1H), 7.41 (t, J=7.9 Hz, 1H), 7.25-7.34 (m, 2H), 3.88 (s, 3H); ES MS (M+1)=260.

WORKUP

后处理

  1. custompurged with hydrogen gas
  2. stirringThe mixture was stirred at ambient temperature under 1 atmosphere of hydrogen gas for 72 hours
  3. filtrationThe mixture was filtered through celite
  4. washthe filter cake was washed with MeOH
  5. customThe filtrate solvent was removed under reduced pressure