HRID1453859

反应详情

EQUATION

反应方程式

HRID 1453859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Benzyloxy-5-methyl-4-oxo-2-[(1,2,3,4-tetrahydro-isoquinolin-2-yl)carbonyl]-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazine (46 mg, 0.110 mmol) was dissolved in a 30% solution of HBr in AcOH, and the reaction was stirred at room temperature for 30 minutes. The solvent was removed in vacuo, and purification of the product was achieved by reverse phase chromatography on a C-18 column using a gradient elution of 95-5% H2O (0.1% TFA)/CH3CN (0.1% TFA). Collection and concentration of the appropriate fractions afforded the title compound. 1H NMR (400 MHz, d6-DMSO) δ 9.88 (s, 1H), 7.24-7.13 (m, 4H), 5.19 (br s, 1H), 4.78 (br s, 1H), 4.37-4.34 (t, 2H), 4.20 (br s, 1H), 3.85 (br s, 1H), 3.76-3.73 (t, 2H), 2.98 (s, 3H), 2.90 (br s, 2H); ES MS (M+1)=327.

WORKUP

后处理

  1. customThe solvent was removed in vacuo, and purification of the product
  2. washa gradient elution of 95-5% H2O (0.1% TFA)/CH3CN (0.1% TFA)
  3. customCollection and concentration of the appropriate fractions