HRID564489

反应详情

EQUATION

反应方程式

HRID 564489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-[({[6-fluoro-3′-(hydroxymethyl)-3-biphenylyl]methyl}amino)-carbonyl]benzoate (0.309 g, 0.786 mmol), lithium hydroxide (0.0282 g, 1.2 mmol), THF (6 mL), and water (2 mL) were combined and stirred under argon at room temperature overnight. Solvents were pumped off, the residue adjusted to pH 2 with 1N HCl, and extracted with EtOAc, washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to afford the title compound as a white solid. LC-MS m/z 379.8 (M+H)+, 1.69 min (ret time); mp 169-171° C.; analytical HPLC shows 93.2% purity, (ret time 7.059 min).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. washwashed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated