HRID637005

反应详情

EQUATION

反应方程式

HRID 637005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.00 g 1-Tert.butoxycarbonyl-azetidin-2(S)-carboxylic acid, 1.70 g 1-amino-6-aminomethyl-isoquinolin, 3.50 g TBTU were dissolved in 40 mL DMF. 3.55 mL N-methylmorpholin was added slowly with stirring. The solution was applied to a reversed-phase chromatography column (lenght 100 mm, diameter 14 mm; Merck Lichroprep RP-18, 15-25 u). Elution was started with 25 mL of methanol/water containing 0.3% acetic acid (10 : 90), then a linear gradient to pure methanol over a period of 75 mL was applied followed by 50 mL of pure methanol. Fraktions of 5 mL each were sampled. The solvent was evaporated to give 3.4 g of the tile compound. MS: 357

WORKUP

后处理

  1. washElution
  2. waita linear gradient to pure methanol over a period of 75 mL was applied followed by 50 mL of pure methanol
  3. aliquotFraktions of 5 mL each were sampled
  4. customThe solvent was evaporated