HRID565609

反应详情

EQUATION

反应方程式

HRID 565609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1′-tert-butoxycarbonyl-spiro[3H-indole-3,4′-piperidin]-2(1H)-one, as described above in Step A, (551 mg, 1.70 mmol) in ethyl acetate saturated with HCl (5 mL) was stirred at ambient temp. for 3 hours as the product salt slowly crystallized out. This salt was collected by filtration and partitioned between methylene chloride and aqueous sat'd. sodium carbonate. The organic layer was separated off, dried (anhyd. sodium sulfate) filtered, and the solvent removed under vacuum. The residue was triturated with diethyl ether to give the title compound as a white solid, mp: 184-186° C.

WORKUP

后处理

  1. customslowly crystallized out
  2. filtrationThis salt was collected by filtration
  3. custompartitioned between methylene chloride and aqueous sat'd
  4. customThe organic layer was separated off
  5. dry with materialdried (anhyd. sodium sulfate)
  6. filtrationfiltered
  7. customthe solvent removed under vacuum
  8. customThe residue was triturated with diethyl ether