Acetic Anhydride → HCID 12838038, Verbindung

HRID 1447113Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1447113
Cl.[Cl:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[CH2:11][NH:10][CH2:9][CH2:8]2.[C:13]([O-])(=[O:15])[CH3:14].[Na+].C(OC(=O)C)(=O)C>C(O)(=O)C>[C:13]([N:10]1[CH2:9][CH2:8][C:7]2[C:12](=[C:3]([Cl:2])[CH:4]=[CH:5][CH:6]=2)[CH2:11]1)(=[O:15])[CH3:14]

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 125950728-Chloro-1,2,3,4-tetrahydroisoquinoline hydrochloride

Produkt 1

HCID 12838038HCID 12838038, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of 20.4 g. (0.1 mole) 8-chloro-1,2,3,4-tetrahydroisoquinoline, hydrochloride, 9.85 g. (0.12 mole) sodium acetate 40 ml. acetic anhydride and 100 ml. acetic acid was heated for 3 hours on a steambath with stirring. After the solvent was removed under reduced pressure, the residue was dissolved in water which was then made basic with concentrated ammonium hydroxide. The crude product was extracted into methylene chloride and the organic solution was washed with water, 10% hydrochloric acid, water and 5% aqueous sodium bicarbonate. The organic solution was then dried over anhydrous magnesium sulfate and then concentrated to dryness under vacuum to afford 2-acetyl-8-chloro-1,2,3,4-tetrahydroisoquinoline as a yellow oil.

Aufarbeitung

  1. additionA mixture of 20.4 g
  2. customAfter the solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in water which
  4. extractionThe crude product was extracted into methylene chloride
  5. washthe organic solution was washed with water, 10% hydrochloric acid, water and 5% aqueous sodium bicarbonate
  6. dry with materialThe organic solution was then dried over anhydrous magnesium sulfate
  7. concentrationconcentrated to dryness under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f382f2d0f52648e1a116ec4774f6ae3b
Quelldatensatz
uspto-grants-1982_02
Patentnummer
US04315935

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