HRID1473349

反应详情

EQUATION

反应方程式

HRID 1473349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 25-mL round-bottom flask was charged with tert-butyl 2-(6-((perfluorophenoxy)sulfonyl)naphthalen-1-yl)pyrrolidine-1-carboxylate (674 mg, 1.240 mmol), DCM (4960 μl), and trifluoroacetic acid (2389 μl, 31.0 mmol) to give a clear, very lightly-colored solution After 1 h, the mixture was concentrated, and the residue was taken up in diethyl ether and sonicated, resulting in the formation of a white solid. The mixture was filtered, and the collected solid was washed with diethyl ether, dried over a stream of N2 (g) for 20 min, then dried under vacuum for 30 min to give perfluorophenyl 5-(pyrrolidin-2-yl)naphthalene-2-sulfonate 2,2,2-trifluoroacetate (647 mg, 1.161 mmol, 94% yield) as a white solid: m/z (ESI) 444.2 (M+H)+.

WORKUP

后处理

  1. customto give a clear, very lightly-colored solution After 1 h
  2. concentrationthe mixture was concentrated
  3. customsonicated
  4. customresulting in the formation of a white solid
  5. filtrationThe mixture was filtered
  6. washthe collected solid was washed with diethyl ether
  7. dry with materialdried over a stream of N2 (g) for 20 min
  8. customdried under vacuum for 30 min