HRID2268071

反应详情

EQUATION

反应方程式

HRID 2268071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 6-ethylspiro[isobenzofuran-1(3H),4′-piperidine]-3-one hydrochloride (53 mg) and phenyl N-(5-phenyl-2-pyrazinyl)carbamate (58 mg) in dimethyl sulfoxide (1 mL) was added 10 M sodium hydroxide aqueous solution (0.02 mL). The mixture was vigorously stirred for 5 minutes followed by partition between water and ethyl acetate. The organic layer was separated and then washed with saturated saline solution and then dried over anhydrous Na2SO4. The concentration of the organic solvent left a residue, which was subjected to the crystallization from ethyl acetate to give the subject compound (46 mg) as crystals (melting point 176-178° C.).

WORKUP

后处理

  1. customby partition between water and ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with saturated saline solution
  4. dry with materialdried over anhydrous Na2SO4
  5. waitThe concentration of the organic solvent left a residue, which
  6. customwas subjected to the crystallization from ethyl acetate