HRID403393

反应详情

EQUATION

反应方程式

HRID 403393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-{3-[(6-chloro-4-o-tolyl-pyridazin-3-yl)-methyl-carbamoyl]-5-methyl-benzenesulfonyl}-butyric acid tert-butyl ester (0.055 g, 89.9 μmol) in dichloromethane (1.5 mL) were added anisole (10.7 mg, 10.8 μL, 98.8 μmol) and trifluoroacetic acid (512 mg, 346 μL, 4.49 mmol) and the light yellow solution was stirred at room temperature for 3.5 hours. The reaction mixture was evaporated to dryness and the residue treated with toluene and again completely evaporated. The product was purified by preparative HPLC (Gemini NX column) using a gradient of methanol:water (containing 0.1% formic acid) (20:80 to 98:2). Colorless foam (0.037 g; 74%). MS (ESI+): m/z=556.09 ([M+H]+).

WORKUP

后处理

  1. customThe reaction mixture was evaporated to dryness
  2. additionthe residue treated with toluene
  3. customagain completely evaporated
  4. customThe product was purified by preparative HPLC (Gemini NX column)