Water → 2,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine

HRID 27889

Reaktionsgleichung

Reaktionsgleichung von HRID 27889
[CH3:1][NH:2][CH2:3][CH:4]1[NH:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[CH2:7][C:6]2[CH:15]=[CH:16][CH:17]=[CH:18][C:5]1=2.C(N(CC)CC)C.O.Br[C:28](Br)([CH3:30])[CH3:29]>>[CH3:1][N:2]1[CH2:30][CH2:28][CH2:29][N:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[CH2:7][C:6]3[CH:15]=[CH:16][CH:17]=[CH:18][C:5]=3[CH:4]2[CH2:3]1

Komponenten

5

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 116582,2-DibromopropaneHCID 130379126,11-Dihydro-N-methyl-5H-dibenz(b,e)azepine-6-methanamine

Produkt 1

HCID 132010192,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine

Versuchsvorschrift

4.76 g 5,6-dihydro-6-methylaminomethyl-11H-dibenzo[b,e]azepine is dissolved in 125 ml dibromopropane and 5 ml triethylamine is added to the solution. The mixture is boiled under reflux with stirring for 2 hours, after which it is cooled. 150 ml Water is then added and the whole is shaken for a little while, after which the aqueous layer is separated from the dibromopropane layer. The organic layer is subsequently dried over sodium sulphate and evaporated to dryness under vacuum. The residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureafter which it is cooled
  3. stirringthe whole is shaken for a little while
  4. customafter which the aqueous layer is separated from the dibromopropane layer
  5. dry with materialThe organic layer is subsequently dried over sodium sulphate
  6. customevaporated to dryness under vacuum
  7. customThe residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent

Quellen und Nachweise

ORD-Eintrag
ord-b9c6f2a81adb4f1a8cfe5312e711565d
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04224321

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