HRID875288

反应详情

EQUATION

反应方程式

HRID 875288 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-phenylpyrrolidine (73.8 g, 0.501 moL) in tetrahydrofuran (500 mL) was added N-bromosuccinimide (124.8 g, 1.4 equivalents) at 20° C. to 30° C., and the mixture was stirred at the same temperature for 4 hr. 1 mol/L Aqueous sodium hydroxide solution (300 mL) was added to the mixture at 27° C., and the mixture was partitioned. The organic layer was dried over anhydrous magnesium sulfate and filtered naturally, and the filtrate was concentrated under reduced pressure. The residue was recrystallized from methanol to give the title compound (97.4 g, brown crystals). yield 86%. melting point 88.1° C.

WORKUP

后处理

  1. customthe mixture was partitioned
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered naturally
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was recrystallized from methanol