HRID507797

反应详情

EQUATION

反应方程式

HRID 507797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a two-neck round bottom flask purged with argon was added successively 4-(1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid (90 mg, 0.24 mmol), dry methanol (1 ml), dry triethyl amine (0.5 ml) and trifluoroethylacetate (1.7 ml). All following procedures were carried on in argon atmosphere. The mixture was stirred for 60 hours. After that the solvents were removed at reduced pressure and the residue was taken up in dry tetrahydrofurane (5 ml). The THF solution was filtered and the solvent removed at reduced pressure. The residue was dried in vacuo for 4 hours to produce 0.54 g of oily compound. MS m/z 623.5 M[C24H27F9N4O5]+1.

WORKUP

后处理

  1. customTo a two-neck round bottom flask purged with argon
  2. customAfter that the solvents were removed at reduced pressure
  3. filtrationThe THF solution was filtered
  4. customthe solvent removed at reduced pressure
  5. customThe residue was dried in vacuo for 4 hours