Reaktion #310561

Reaktionsgleichung

dichloromethane

lithium hydride

product

1-pentanoylaminomethyl-1-ethyl-indolo(2,3-a)quinolizidine

water

→

oil

Ausbeute 98.3%

1-pentylaminomethyl-1-ethyl-indolo(2,3-a)quinolizidine

Ausbeute 98.3%

Lösungsmittel

ethyl ether

ethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn a 500 ml three-necked flask of having
2. 2
   Sonstigea stirrer, a reflux condenser, a thermometer, and a dropping funnel there were placed
3. 3
   TemperaturWhen this had been cooled on an ice bath
4. 4
   TemperaturThe mixture was then heated
5. 5
   Temperaturunder reflux for 2 hours
6. 6
   workup.STIRRINGstirred for a further 15 hours at room temperature
7. 7
   TemperaturIt was then cooled on an ice bath
8. 8
   FiltrationThe mixture was then filtered over Celite
9. 9
   Trocknendried over sodium sulphate
10. 10
    Einengenconcentrated by evaporation

Vorschrift

In a 500 ml three-necked flask of having a stirrer, a reflux condenser, a thermometer, and a dropping funnel there were placed 100 ml of anhydrous ethyl ether. When this had been cooled on an ice bath there were added 4 g of lithium hydride, and the contents of the flask were stirred for 15 minutes. There was then added very slowly a solution of 7.4 g of the product of Example 7 in 50 ml of anhydrous ethyl ether. The mixture was then heated under reflux for 2 hours and stirred for a further 15 hours at room temperature. It was then cooled on an ice bath and there were added dropwise 20 ml of water followed by 150 ml of dichloromethane. The mixture was then filtered over Celite, dried over sodium sulphate and concentrated by evaporation. There were obtained 7 g of an oil which could be crystallized to a product melting at 80° C.

Quelle