HRID44146

反应详情

EQUATION

反应方程式

HRID 44146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (S)-2-(tert-butoxycarbonylamino)-3,3-dimethylbutanoic acid (18) (6.5 g, 19.7 mmol) in THF (30 mL) was added NaOH (1.7 g, 43.8 mmol) in H2O (60 mL) and the reaction mixture stirred at ambient temperature for 16 h. THF was subsequently removed in vacuo and the aqueous phase washed with EtOAc (50 mL). The aqueous phase was then adjusted to pH ˜2 by addition of 1M HCl and extracted with EtOAc (3×50 mL). The organics were combined dried over MgSO4 and evaporated to give the desired compound (20) as a white solid (5.7 g, 95%); AnalpH2_MeOH; Rt 2.61 min; m/z 303 (MH+); white solid

WORKUP

后处理

  1. customTHF was subsequently removed in vacuo
  2. washthe aqueous phase washed with EtOAc (50 mL)
  3. additionThe aqueous phase was then adjusted to pH ˜2 by addition of 1M HCl
  4. extractionextracted with EtOAc (3×50 mL)
  5. dry with materialThe organics were combined dried over MgSO4
  6. customevaporated