HRID894217
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- dissolutionDissolve 450 mg
- customEvaporate the alcohol
- additiondilute the residual sodium salt solution with 40 ml of water
- temperatureCool in an ice bath
- customSeparate the solids
- filtrationby filtration
- customdry (yield 250 mg)
- customRecrystallize from benzene