Tetrahydrofuran → HCID 178515336, Verbindung

HRID 485463Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 485463
O1CCCC1.[Cl-].[Al+3].[Cl-].[Cl-].[C:10]([CH2:12][C:13]1[CH:14]=[CH:15][C:16]2[C:22](=[O:23])[CH2:21][C:20]3[CH:24]=[CH:25][CH:26]=[CH:27][C:19]=3[S:18][C:17]=2[CH:28]=1)#[N:11].[N-:29]=[N+:30]=[N-:31].[Na+]>O>[NH:29]1[C:10]([CH2:12][C:13]2[CH:14]=[CH:15][C:16]3[C:22](=[O:23])[CH2:21][C:20]4[CH:24]=[CH:25][CH:26]=[CH:27][C:19]=4[S:18][C:17]=3[CH:28]=2)=[N:11][N:31]=[N:30]1

Komponenten

6

Edukt 4

HCID 8028TetrahydrofuranHCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 202702303-Cyanomethyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin

Produkt 1

HCID 178515336HCID 178515336, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Add to 25 cc. of tetrahydrofuran cooled in an ice bath 1.59 gm. (11.9 mmole) of aluminum chloride, 1.33 gm. (5.25 mmole) of 3-cyanomethyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin and 1.55 gm. (23.8 mmole) of sodium azide. Reflux the mixture for 19 hours, cool, dilute with water and acidify. Extract the mixture into ethyl acetate and evaporate. Triturate the residue in ether and separate the title product by filtration.

Aufarbeitung

  1. additionAdd to 25 cc
  2. temperatureReflux the mixture for 19 hours
  3. temperaturecool
  4. extractionExtract the mixture into ethyl acetate
  5. customevaporate
  6. customTriturate the residue in ether
  7. customseparate the title product
  8. filtrationby filtration

Quellen und Nachweise

ORD-Eintrag
ord-7c4e25b67a7a4dcc8b4ba67bdf143ab1
Quelldatensatz
uspto-grants-1985_08
Patentnummer
US04536507

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