HRID1810368

反应详情

EQUATION

反应方程式

HRID 1810368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To 2-{2′-[(acetyl-ethyl-amino)-methyl]-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl}-2-methyl-propionic acid ethyl ester (0290 g, 0.63 mmol) in THF (2.6 mL) and EtOH (2 mL) was added 1N aqueous NaOH (1.9 mL), and the reaction was stirred at 50° C. overnight. Analytical LCMS indicated that starting material was still present, so additional 1N aqueous NaOH (1 mL) was added, and the reaction was stirred at 70° C. for 2 hours. Additional 1N aqueous NaOH (1 mL) was added, and the reaction was stirred for another 6 hours. The mixture was worked-up with CH2Cl2 and 1N aqueous HCl, and the organic layer was dried over Na2SO4, decanted, and concentrated. The residue was purified by preparative HPLC to give the title compound. M+H is 438.

WORKUP

后处理

  1. stirringthe reaction was stirred at 70° C. for 2 hours
  2. stirringthe reaction was stirred for another 6 hours
  3. dry with materialthe organic layer was dried over Na2SO4
  4. customdecanted
  5. concentrationconcentrated
  6. customThe residue was purified by preparative HPLC