Reaktion #218598

Reaktionsgleichung

3-methyl-5H-dibenzo[b,e][1,4]diazepin-1-ylamine hydrochloride

(S)-2-(2-methoxy-ethyl)-piperazine

N,N-diisopropylethylamine

DMSO

→

yellow foam

Ausbeute 48.0%

(S)-3-Methyl-11-[3-(2-methoxy-ethyl)-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine

Ausbeute 48.0%

Lösungsmittel

toluene

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcool the mixture to ambient temperature
2. 2
   WaschenWash the organic layer with 0.1N NaOH and brine
3. 3
   TrocknenDry (sodium sulfate)
4. 4
   Einengenconcentrate the organic layer to residue
5. 5
   SonstigePurify the residue on silica gel

Vorschrift

Combine 3-methyl-5H-dibenzo[b,e][1,4]diazepin-1-ylamine hydrochloride (400.0 mg, 1.54 mmol), (S)-2-(2-methoxy-ethyl)-piperazine (444.2 mg, 3.08 mmol), N,N-diisopropylethylamine (199.0 mg, 1.54 mmol), DMSO (0.7 ml), and toluene (2.8 ml) and stir and heat the mixture at 110° C. After 48 hours, cool the mixture to ambient temperature and dilute with ethyl acetate. Wash the organic layer with 0.1N NaOH and brine. Dry (sodium sulfate) and concentrate the organic layer to residue. Purify the residue on silica gel using dichloromethane/methanol (90:10) to give 257.1 mg (48%) of a yellow foam: mp=64° C. dec; mass spectrum (ion spray): m/z =433.1 (M+1).

Quelle