Ammonium Hydroxide → HCID 178511888, Verbindung

HRID 2296619Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2296619
Cl.[O:2]1[C:8]2[CH:9]=[CH:10][C:11]([NH2:13])=[CH:12][C:7]=2[CH2:6][NH:5][CH2:4][CH2:3]1.I.[S:15]1[CH:19]=[CH:18][C:17]([C:20](SC)=[NH:21])=[CH:16]1.[OH-].[NH4+]>C(O)C.O>[O:2]1[C:8]2[CH:9]=[CH:10][C:11]([NH:13][C:20]([C:17]3[CH:18]=[CH:19][S:15][CH:16]=3)=[NH:21])=[CH:12][C:7]=2[CH2:6][NH:5][CH2:4][CH2:3]1

Komponenten

6

Edukt 3

HCID 14923Ammonium HydroxideHCID 18387495HCID 18387495, VerbindungHCID 131722237HCID 131722237, Verbindung

Produkt 1

HCID 178511888HCID 178511888, VerbindungAusbeute 22,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-ylamine hydrochloride (1.84 g, 8.4 mmol) was dissolved in 95% ethanol (40 ml) and 3-thiophenecarboximidothioic acid, methyl ester, hydroiodide (2.85 g, 10 mmol) was added. The mixture was stirred at room temperature for 2 days and then heated at 60° C. overnight and cooled. The solid (1.02 g) was collected. The filtrate was evaporated and the residue treated with ethyl acetate. The resulting crystals were collected and combined with the solid obtained previously. They were dissolved in water (20 ml), basified with conc. ammonium hydroxide, and extracted with methylene chloride (3×30 ml). The organic extracts were washed with water, dried over magnesium sulfate, and concentrated to give a solid (0.508 g), m.p. 150-152° C.

Aufarbeitung

  1. temperatureheated at 60° C. overnight
  2. temperaturecooled
  3. customThe solid (1.02 g) was collected
  4. customThe filtrate was evaporated
  5. additionthe residue treated with ethyl acetate
  6. customThe resulting crystals were collected
  7. customobtained previously
  8. extractionextracted with methylene chloride (3×30 ml)
  9. washThe organic extracts were washed with water
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8c246586e3974b0fb63ec0a03b399b85
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06489322B1

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