HRID333065

反应详情

EQUATION

反应方程式

HRID 333065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(E)-4,4,5,5,5-Pentafluoropent-2-enoic acid (38 mg, 0.2 mmol) and HBTU (76 mg, 0.2 mmol) were dissolved in a 1:1 mixture of anhydrous DMF and anhydrous acetonitrile (2 ml), after 5 minutes triethylamine (82 μl, 0.6 mmol) and N-(2-methyl-4-quinolyl)propane-1,3-diamine hydrochloride (48 mg, 0.24 mmol) was added and stirring was continued for 3 hours. To the mixture basic aluminium oxide was added, stirring was continued for one hour, the mixture was filtered and the filtrate was evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 28.4 mg (0.076 mmol, 38%).

WORKUP

后处理

  1. additionwas added
  2. stirringstirring
  3. waitwas continued for one hour
  4. filtrationthe mixture was filtered
  5. customthe filtrate was evaporated to dryness under reduced pressure
  6. customThe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
  7. customto yield 28.4 mg (0.076 mmol, 38%)