HRID1755481

反应详情

EQUATION

反应方程式

HRID 1755481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution material from Example 97 (4.7 g, 9.10 mmol) in anhydrous DMF (30 mL) is added piperidine (15 mL, 152 mmol). The resulting solution is stirred at room temp for 45 rain and the solvent is removed in vacuo. The resulting residue was redissolved in 1,4-dioxane (50 mL), the solvent was removed in vacuo again and the resulting solid was dried under high vacuum for 18 h to give the title compound as a white solid in quantitative yield that contains 1 equivalent of 1-((9H-fluoren-9-yl)methyl)piperidine as a side product. LC/MS (Condition A): ret. T=2.30 rain, (M+H)+ 295.

WORKUP

后处理

  1. customthe solvent is removed in vacuo
  2. dissolutionThe resulting residue was redissolved in 1,4-dioxane (50 mL)
  3. customthe solvent was removed in vacuo again
  4. customthe resulting solid was dried under high vacuum for 18 h