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Triethylamine → 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

HRID 2308936
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2308936
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][CH2:8][C:7](=[O:11])[C:6]=2[CH:12]=1.CO[CH:15](OC)[N:16]([CH3:18])[CH3:17].C(N(CC)CC)C>C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8](=[CH:15][N:16]([CH3:18])[CH3:17])[C:7](=[O:11])[C:6]=2[CH:12]=1
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Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 2480656-Chlorothiochroman-4-one

Produkt 1

HCID 38135366-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A solution of 6-chloro-2,3-dihydro-4H-1-benzothiopyran-4-one (30 g), N,N-dimethylformamide dimethyl acetal (80 ml), and triethylamine (31.4 ml) in benzene (400 ml) was refluxed with stirring for 1 hour and then about three-fourths of the solvent were distilled slowly at atmospheric pressure over a period of approximately 1 hour. Benzene (300 ml) was added to the reaction mixture and the solvent was distilled again. To the residue was added diethyl ether (150 ml) and the mixture was triturated to give 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one (34 g).

Aufarbeitung

  1. distillationabout three-fourths of the solvent were distilled slowly at atmospheric pressure over a period of approximately 1 hour
  2. additionBenzene (300 ml) was added to the reaction mixture
  3. distillationthe solvent was distilled again
  4. additionTo the residue was added diethyl ether (150 ml)
  5. customthe mixture was triturated

Quellen und Nachweise

ORD-Eintrag
ord-e9d86e1fce0949b381afb289ab19606f
Quelldatensatz
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04692444

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