Reaktion #40392

Reaktionsgleichung

ethyl 4-(4-{2-[2-(6-benzyloxy-3-oxo-3,4-dihydro-2H-benzo [1,4]oxazin-8-yl)-2-hydroxyethylamino]-2-methylpropyl}phenoxy)butyrate

sodium hydroxide

hydrochloric acid

→

4-(4-{2-[2-(6-benzyloxy-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl)2-hydroxyethylamino]-2-methylpropyl}phenoxy)butyric acid

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 30 minutes
2. 2
   SonstigeThe solution is evaporated down
3. 3
   workup.DISSOLUTIONthe residual oil is dissolved
4. 4
   Temperaturby heating in 5 mL of n-butanol
5. 5
   workup.ADDITIONAfter the addition of a crystallization aid
6. 6
   Sonstigea solid is precipitated out which
7. 7
   Filtrationfiltered
8. 8
   Waschenwashed with acetone and diethyl ether

Vorschrift

A solution of 1.00 g (1.73 mmol) of ethyl 4-(4-{2-[2-(6-benzyloxy-3-oxo-3,4-dihydro-2H-benzo [1,4]oxazin-8-yl)-2-hydroxyethylamino]-2-methylpropyl}phenoxy)butyrate in 25 mL methanol is combined with 2.5 mL of 1 N sodium hydroxide solution, refluxed for 30 minutes, and then neutralized with 1 N hydrochloric acid. The solution is evaporated down and the residual oil is dissolved by heating in 5 mL of n-butanol. After the addition of a crystallization aid, a solid is precipitated out which is suction filtered and washed with acetone and diethyl ether. Yield: 0.75 g (79%); melting point: 216° C.-218° C.

Quelle