Bromine → HCID 20374951, Verbindung

HRID 1448993

Reaktionsgleichung

Reaktionsgleichung von HRID 1448993
[Na].[CH2:2]([O:9][C:10]1[CH2:14][CH:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.BrBr.[CH3:25][NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>C(O)CCCCCC.C1C=CC=CC=1>[CH2:27]([N:26]([CH3:25])[CH:12]1[CH:11]([O:9][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH:10]([O:9][CH2:2][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:14][CH:13]1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]

Komponenten

7

Edukt 4

HCID 24408BromineHCID 93190N-MethylheptylamineHCID 5360545SodiumHCID 20374931HCID 20374931, Verbindung

Produkt 1

HCID 20374951HCID 20374951, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittel2×HCID 8129HeptanolLösungsmittel

Versuchsvorschrift

0.23 g of sodium are dissolved in 30 ml of 1-heptanol at 50° under nitrogen. Dropwise, with stirring, there is added 4.88 g of N-heptyl-N-methyl-2-bromo-4,5-bibenzyloxycyclopentane-1-amine (obtainable from 3,5-dibenzyloxy-2-cyclopentene by the addition of bromine and reaction with 1-equivalent of methyl heptylamine), dissolved in 30 ml of benzene. Stirring is carried on for 6 hours at 50°. After cooling, 100 ml of benzene is added thereto. This is washed with water. The organic phase is dried over MgSO4 and the solvent is distilled off. After chromatographic purification of the residue (silica gel/chloroform:acetone=9:1), N-heptyl-N-methyl-5-heptyloxy-2,4-dibenzyloxy-cyclopentane-1-amine is obtained.

Aufarbeitung

  1. stirringStirring
  2. customis carried on for 6 hours at 50°
  3. temperatureAfter cooling
  4. washThis is washed with water
  5. dry with materialThe organic phase is dried over MgSO4
  6. distillationthe solvent is distilled off
  7. customAfter chromatographic purification of the residue (silica gel/chloroform:acetone=9:1)

Quellen und Nachweise

ORD-Eintrag
ord-94ef12ff946346dc905bfdf4177f9e32
Quelldatensatz
uspto-grants-1980_02
Patentnummer
US04188403

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