HRID1437357

反应详情

EQUATION

反应方程式

HRID 1437357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of (a) (630 mg, 2.8 mmol) in DMF (10 ml) was treated with trifluoroacetic acid anhydride (4 ml). The clear solution was stirred at room temperature overnight then evaporated. The residue was treated with dilute aqueous sodium carbonate solution and extracted several times with 5% methanol/dichloromethane. The combined organic extracts were washed with brine, dried and evaporated. The crude product was chromatographed on silica eluting with 0-10% methanol in dichloromethane affording a white solid (180 mg, 29%).

WORKUP

后处理

  1. customthen evaporated
  2. additionThe residue was treated with dilute aqueous sodium carbonate solution
  3. extractionextracted several times with 5% methanol/dichloromethane
  4. washThe combined organic extracts were washed with brine
  5. customdried
  6. customevaporated
  7. customThe crude product was chromatographed on silica eluting with 0-10% methanol in dichloromethane affording a white solid (180 mg, 29%)