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Triethylamine → (+)-8-Chloro-6,11-dihydro-11-[4-(4-pyridinylmethyl)-1-piperazinyl]-5h-benzo[5,6]cyclohepta-[1,2-b]pyridine

HRID 21416
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 21416
[CH:1]1[C:6]([CH2:7]O)=[CH:5][CH:4]=[N+:3]([O-])[CH:2]=1.C(Br)(Br)(Br)Br.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:34][C:35]1[CH:36]=[CH:37][C:38]2[CH:48]([N:49]3[CH2:54][CH2:53][NH:52][CH2:51][CH2:50]3)[C:43]3=[N:44][CH:45]=[CH:46][CH:47]=[C:42]3[CH2:41][CH2:40][C:39]=2[CH:55]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:34][C:35]1[CH:36]=[CH:37][C:38]2[CH:48]([N:49]3[CH2:50][CH2:51][N:52]([CH2:7][C:6]4[CH:5]=[CH:4][N:3]=[CH:2][CH:1]=4)[CH2:53][CH2:54]3)[C:43]3=[N:44][CH:45]=[CH:46][CH:47]=[C:42]3[CH2:41][CH2:40][C:39]=2[CH:55]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 8471TriethylamineHCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 896664-Pyridylmethanol N-oxideHCID 5255691HCID 5255691, Verbindung

Produkt 1

HCID 19933864(+)-8-Chloro-6,11-dihydro-11-[4-(4-pyridinylmethyl)-1-piperazinyl]-5h-benzo[5,6]cyclohepta-[1,2-b]pyridine
Ausbeute 45,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a mixture of 188 mg (1.50 mmol) of 4-pyridylcarbinol N-oxide and 497 mg (1.50 mmol) of carbon tetrabromide in 12 mL of dry methylene chloride at room temperature and under an argon atmosphere was added in one portion 393 mg (1.50 mmol) of triphenylphosphine. After 40 minutes, 313 mg (0.997 mmol) of (-)-8-chloro-6,11-dihydro-11-(4-piperazinyl)-5H-benzo[5,6]cyclohepta-[1,2-b]pyridine was added followed by 209 mL (1.57 mmol) of triethylamine. The reaction mixture was then allowed to stir at room temperature for 3 hr, after which it was taken up in methylene chloride and washed once with 0.5M aqueous sodium bicarbonate and then brine. The organic portion was dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified via flash chromatography (4% methanol saturated with ammonia in methylene chloride) to provide 183 mg of (-)-8-chloro-6,11-dihydro-11-[4 -(4-pyridinylmethyl)-1-piperazinyl]-5h-benzo[5,6]cyclohepta-[1,2-b]pyridine, N-oxide as a glass: MS (CI) m/z 421 (M+ +1);

Aufarbeitung

  1. washwashed once with 0.5M aqueous sodium bicarbonate
  2. dry with materialThe organic portion was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified via flash chromatography (4% methanol saturated with ammonia in methylene chloride)

Quellen und Nachweise

ORD-Eintrag
ord-1ba716dc820347e494732209b62094f7
Quelldatensatz
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05422351

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