Reaktion #1856735

Reaktionsgleichung

Ethyl α-amino-5H-dibenzo[a,d]cycloheptene-5-acetate, hydrochloride

potassium hydroxide

hexane

2-propanol

→

α-Amino-5H-dibenzo[a,d]cycloheptene-5-acetic acid, hydrochloride

Lösungsmittel

water

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeno starting material (2 hours)
2. 2
   Extraktionextracted with dichloromethane
3. 3
   workup.ADDITIONThe residue is treated with 5 mL of boiling water
4. 4
   Sonstigerefrigerated overnight
5. 5
   SonstigeA solid is collected
6. 6
   Waschenwashed with diethyl ether (0.05 g)

Vorschrift

Ethyl α-amino-5H-dibenzo[a,d]cycloheptene-5-acetate, hydrochloride (0.21 g, 0.6 mmol) dissolved in 10 mL of absolute ethanol is stirred with 3 mL of 1.25M ethanolic potassium hydroxide solution until TLC (SiO2, hexane: 2-propanol/3: 1) shows no starting material (2 hours). The solvent is stripped and a residual solid is taken up in water and extracted with dichloromethane. The aqueous layer is acidified with 6N hydrochloric acid to pH 1 and stripped to dryness. The residue is treated with 5 mL of boiling water, cooled to room temperature, then refrigerated overnight. A solid is collected, washed with diethyl ether (0.05 g); mp 225° C. (dec).

Quelle