반응 #592795

반응 방정식

methyl 4-{[{2-[(2-chlorobenzyl)-oxy]phenethyl}(5-methoxy-5-oxopentyl)amino]methyl}benzoate

water

sodium hydroxide

→

4-[((4-carboxybutyl){2-[(2-chlorobenzyl)oxy]phenethyl}amino)methyl]-benzoic Acid

용매

methanol

반응 조건

후처리

1. 1
   온도cooled
2. 2
   workup.DISTILLATIONthe methanol is distilled off under reduced pressure
3. 3
   workup.ADDITIONThe aqueous phase is adjusted to pH 4 by addition of a citric acid/aqueous sodium hydroxide solution buffer
4. 4
   기타the resulting precipitate is separated off
5. 5
   기타Tituration with boiling cyclohexane gives a finely crystalline product

실험 절차

124.8 mg (0.238 mmol) of methyl 4-{[{2-[(2-chlorobenzyl)-oxy]phenethyl}(5-methoxy-5-oxopentyl)amino]methyl}benzoate from Ex. 1 are initially charged in 0.3 ml of methanol and 0.17 ml of water and admixed with 0.2 ml of a 40% strength sodium hydroxide solution. The mixture is stirred at 60° C. for one hour and then cooled, and the methanol is distilled off under reduced pressure. The aqueous phase is adjusted to pH 4 by addition of a citric acid/aqueous sodium hydroxide solution buffer and the resulting precipitate is separated off. Tituration with boiling cyclohexane gives a finely crystalline product.

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