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Sodium → 7-benzyl-4-phenyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine

HRID 239114
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 239114
[Na].Cl.[CH:3]([NH2:5])=[NH:4].[CH2:6]([N:13]1[CH2:19][CH2:18][C:17](Cl)=[C:16]([C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=O)[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[CH2:6]([N:13]1[CH2:14][CH2:15][C:16]2[C:21]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[N:4][CH:3]=[N:5][C:17]=2[CH2:18][CH2:19]1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 5360545SodiumHCID 10313058Methanimidamide, hydrochloride (1:1)HCID 69190815(1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanone

Produkt 1

HCID 866860407-benzyl-4-phenyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepineAusbeute 39,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702Ethanol
Lösungsmittel

Reaktionsbedingungen

Temperatur
6 °C

Versuchsvorschrift

16.8 g sodium was added to 500 mL ethanol at 10° C. Then, 48.5 g formamidine hydrochloride was added and the reaction was stirred 15 min at 6° C. 28 g (1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanone was added and the reaction was stirred 17 h at RT and 1 h at 40° C. The mixture was filtered and the solvent was removed. The residue was dissolved in ethyl acetate. The layers were separated and the organic layer was washed with water and evaporated. The residue was crystallized with diethylether to yield 10.7 g of the desired product. Fp: 81-82° C.

Aufarbeitung

  1. stirringthe reaction was stirred 17 h at RT and 1 h at 40° C
  2. filtrationThe mixture was filtered
  3. customthe solvent was removed
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. customThe layers were separated
  6. washthe organic layer was washed with water
  7. customevaporated
  8. customThe residue was crystallized with diethylether

Quellen und Nachweise

ORD-Eintrag
ord-5080a0aef6f745e6b0f5a947c25647a3
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08642774B2

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