HRID894217

反应详情

EQUATION

反应方程式

HRID 894217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 450 mg. of methyl 11-hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate in 20 ml. of ethanol and add 20 ml. of 5% aqueous sodium hydroxide solution. Stir at room temperature for 1 hour. Evaporate the alcohol and dilute the residual sodium salt solution with 40 ml of water. Cool in an ice bath and acidify with 5N hydrochloric acid. Separate the solids by filtration and dry (yield 250 mg). Recrystallize from benzene to obtain the title product (yield 200 mg., m.p. 258°-258° C.).

WORKUP

后处理

  1. dissolutionDissolve 450 mg
  2. customEvaporate the alcohol
  3. additiondilute the residual sodium salt solution with 40 ml of water
  4. temperatureCool in an ice bath
  5. customSeparate the solids
  6. filtrationby filtration
  7. customdry (yield 250 mg)
  8. customRecrystallize from benzene