HRID1054175

反应详情

EQUATION

反应方程式

HRID 1054175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 7-bromo-3-(2-ethoxy-2-oxoethyl)-2,3-dihydro-4H-1,4-benzoxazine-4-carboxylate (Intermediate 24, 556 mg, 1.39 mmol) was dissolved in hydrogen chloride in dioxane (5.0 mL, 162.8 mmol) and the mixture stirred for 2 h at rt. The solvent was evaporated and the residue dissolved in EtOAc (50 mL), washed with sat. aq. Na2CO3 (30 mL) and brine (20 mL), dried over Na2SO4 and evaporated after filtration to give the title compound (399 mg, 96%) as an oil.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in EtOAc (50 mL)
  3. washwashed with sat. aq. Na2CO3 (30 mL) and brine (20 mL)
  4. dry with materialdried over Na2SO4
  5. customevaporated
  6. filtrationafter filtration