HRID2255641

反应详情

EQUATION

反应方程式

HRID 2255641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 929 mg (2.24 mmol) of the product of Step L in benzene were added oxalyl chloride (234 mL, 2.69 mmol) and one drop of DMF at 0° C. The solution was stirred at rt for 45 minutes. After concentration the residue was dissolved in CH2Cl2 (10 mL). The solution was added to a solution of tert-butyl alcohol (253 mL, 2.69 mmol) and Et3N in CH2Cl2 (10 mL) at 0° C. The solution was stirred at rt for 3 hours. The mixture was poured into EtOAc (50 mL) and washed with H2O (1×) and brine, and dried over anhydrous MgSO4. Concentration gave 778 mg of the title compound as a slightly yellow glass.

WORKUP

后处理

  1. concentrationAfter concentration the residue
  2. dissolutionwas dissolved in CH2Cl2 (10 mL)
  3. stirringThe solution was stirred at rt for 3 hours
  4. washwashed with H2O (1×) and brine
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationConcentration