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Hydrochloric Acid → HCID 178526950, Verbindung

HRID 1004414
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1004414
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15](Br)=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:19][C:20]1[C:29]2[O:28][C:27]([C:30]3[NH:34][N:33]=[N:32][N:31]=3)=[CH:26][C:25](=[O:35])[C:24]=2[CH:23]=[CH:22][CH:21]=1.N12CCCN=C1CCCCC2.Cl.[C:48]([O-])(=[O:50])C.[Na+]>CN1CCCC1=O.O.CO.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[OH2:11].[O:35]=[C:25]1[C:24]2[CH:23]=[CH:22][CH:21]=[C:20]([NH:19][C:48](=[O:50])[C:15]3[CH:16]=[CH:17][C:12]([O:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:13][CH:14]=3)[C:29]=2[O:28][C:27]([C:30]2[NH:34][N:33]=[N:32][N:31]=2)=[CH:26]1.[O:35]=[C:25]1[C:24]2[CH:23]=[CH:22][CH:21]=[C:20]([NH:19][C:48](=[O:50])[C:15]3[CH:16]=[CH:17][C:12]([O:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:13][CH:14]=3)[C:29]=2[O:28][C:27]([C:30]2[NH:34][N:33]=[N:32][N:31]=2)=[CH:26]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 517045Sodium AcetateHCID 108704574-(4-Phenylbutoxy)bromobenzeneHCID 178507421HCID 178507421, Verbindung

Produkt 1

HCID 178526950HCID 178526950, Verbindung
Ausbeute 78,7 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 6102075Dichlorobis(triphenylphosphine)palladiumKatalysatorHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Versuchsvorschrift

A mixture of 4-(4-phenylbutoxy)bromobenzene (0.50 g, 1.64 mmole), 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran (0.75 g, 3.28 mmole), bis-(triphenylphospine)palladium (II) chloride (0.135 g, 0.19 mmole) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.87 g, 5.74 mmole) was stirred in N-methylpyrrolidinone (10 ml) at 100-110° C. under an atmosphere of carbon monoxide at atmospheric pressure for 4.5 hours. The reaction mixture was diluted with water (15 ml) and acidified using concentrated hydrochloric acid (5 ml). The precipitate was filtered, washed with water and methanol and then stirred in concentrated hydrochloric acid (8 ml) to dissolve unreacted 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran. The undissolved solid was filtered, washed with concentrated hydrochloric (2×1.5 ml), water, then methanol. The damp cake was stirred with sodium acetate (0.15 g, 1.83 mmole) in methanol (10 ml) and the solution filtered. The supernatant liquor was acidified with concentrated hydrochloric acid (0.2 ml), and the product filtered, washed with methanol and dried to give the title compound (422 mg, 53%).

Aufarbeitung

  1. filtrationThe precipitate was filtered
  2. washwashed with water and methanol
  3. dissolutionto dissolve unreacted 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran
  4. filtrationThe undissolved solid was filtered
  5. washwashed
  6. concentrationwith concentrated hydrochloric (2×1.5 ml), water
  7. filtrationthe solution filtered
  8. filtrationthe product filtered
  9. washwashed with methanol
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-20dfe70612ba4bf2a79bedfcee9a97cc
Quelldatensatz
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06048983

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