Reaktion #11668

Reaktionsgleichung

3-acetamidoamino-3-carboethoxy-5-methoxy-3,4-dihydrocarbostyril

hydrochloric acid

→

3-amino-5-methoxy-3,4-dihydrocarbostyril hydrochloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 6 h
2. 2
   SonstigeThis mixture was evaporated to a solid which
3. 3
   Sonstigewas triturated with acetonitrile
4. 4
   FiltrationFiltration

Vorschrift

A mixture of 3-acetamidoamino-3-carboethoxy-5-methoxy-3,4-dihydrocarbostyril (5.7 g) and 6 M aqueous hydrochloric acid (75 mL) was refluxed for 6 h. This mixture was evaporated to a solid which was triturated with acetonitrile. Filtration provided 3-amino-5-methoxy-3,4-dihydrocarbostyril hydrochloride (3.8 g, mp 301–302° C. with decomp.) as gray crystals. The free base, 3-amino-5-methoxy-3,4-dihydrocarbostyril, was prepared by ion exchange on an SCX column (United Chemical Technologies, CLEAN-UP Extraction Column, sorbent CUBCX1HL, Synthesis 1997, 553–558) by loading in methanol and eluting with methanol, followed by 2 M methanolic ammonia. The ammonia containing eluant was evaporated to provide 3-amino-5-methoxy-3,4-dihydrocarbostyril.

Quelle