HRID873810

反应详情

EQUATION

反应方程式

HRID 873810 的结构方程式

PROCEDURE

实验过程

The title compound was prepared in analogy to the procedure described in Step 10.3 using ethyl 4-((4-chlorophenyl)(hydroxy)methyl)-1-methyl-1H-pyrazole-3-carboxylate (Step 10.2) and 5-amino-1,3-dimethylpyridin-2(1H)-one (Step 20.2). After purification by silica gel column chromatography, the resulting residue was further purified by preparative HPLC (Gilson gx-281; column: Sunfire C18, 30×100 mm, 5 μm; flow: 30 mL/min; gradient: 5% to 100% B in 20 min; A=0.1% TFA in H2O, B=CH3CN. detection: UV). tR: 3.91 min (HPLC 1); tR: 0.90 min (LC-MS 2); ESI-MS: 415 [M+H]+ (LC-MS 2); Rf=0.46 (CH2Cl2/MeOH 9:1).

WORKUP

后处理

  1. customAfter purification by silica gel column chromatography
  2. customthe resulting residue was further purified by preparative HPLC (Gilson gx-281