HRID261476

反应详情

EQUATION

反应方程式

HRID 261476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.4 g of 2,3-dihydro-1'-acetyl-5-nitrospiro[benzofuran-2,4'-piperidine] in 150 ml of 6 N hydrochloric acid is refluxed for 45 hours and then stirred at ambient temperature for 16 hours. Thereafter, the reaction mixture is successively extracted once with ether, basified with 6 N sodium hydroxide and extracted thrice with ether. The combined ether extracts are dried and the solvent removed, leaving a yellow residue. The residue is dissolved in ether where it is converted to its hydrogen chloride salt. The salt is collected, dried and finally recrystallized twice from ethyl alcohol to give the product 2,3-dihydro-5-nitrospiro[benzofuran-2,4'-piperidine]hydrochloride, mp 265°-266° C.

WORKUP

后处理

  1. extractionThereafter, the reaction mixture is successively extracted once with ether
  2. extractionextracted thrice with ether
  3. dry with materialThe combined ether extracts are dried
  4. customthe solvent removed
  5. customleaving a yellow residue
  6. customThe salt is collected
  7. customdried
  8. customfinally recrystallized twice from ethyl alcohol