HRID1026205

反应详情

EQUATION

反应方程式

HRID 1026205 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl [(1S)-2-({6-[6-(cyclopropylmethoxy)-1,3-benzoxazol-2-yl]pyridin-3-yl}oxy)-1-methylethyl]carbamate (350 mg) in ethyl acetate (20 mL) was added 4M hydrogen chloride/ethyl acetate (10 mL), and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure, and the residue was dissolved in pyridine (15 mL). Acetic anhydride (163 mg) was added thereto, and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol), and recrystallized (hexane/ethyl acetate) to give the title compound (201 mg).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in pyridine (15 mL)
  3. additionAcetic anhydride (163 mg) was added
  4. stirringthe mixture was stirred at room temperature for 15 hr
  5. concentrationThe reaction mixture was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol)
  7. customrecrystallized (hexane/ethyl acetate)