HRID54618

反应详情

EQUATION

反应方程式

HRID 54618 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from Example 8 (3.78 g; 13 mmol) and N-(fluorenylmethyloxycarbonyl)glycine (5.9 g; 20 mmol) are dissolved in anhydrous N,N-dimethylformamide (160 ml) under a protective atmosphere of argon gas. N,N'-Dicyclohexylcarbodiimide (4.11 g; 20 mmol) is added in portions at 0° C. The mixture is stirred at room temperature for 21 h and the solid which has precipitated is subsequently filtered off with suction. The solution is then concentrated in vacuo, and subsequently distilled repeatedly with toluene, and the crude product is chromatographed on silica gel. (Eluent: toluene/ethanol, 30:1-20:1). Yield: 6.33 g (82%).

WORKUP

后处理

  1. customthe solid which has precipitated
  2. filtrationis subsequently filtered off with suction
  3. concentrationThe solution is then concentrated in vacuo
  4. distillationsubsequently distilled repeatedly with toluene
  5. customthe crude product is chromatographed on silica gel