Sulfuric Acid → N-methyl-2H-3-isoquinolone

HRID 1075818

Reaktionsgleichung

Reaktionsgleichung von HRID 1075818
[CH:1]([N:3]([CH3:13])[C:4](=[O:12])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=O.S(=O)(=O)(O)O.S(O)(O)(=O)=O.CN1C(=O)C=C2C(C=CC=C2)=C1>C(O)C>[CH3:1][N:3]1[C:4](=[O:12])[CH:5]=[C:6]2[C:11]([CH:10]=[CH:9][CH:8]=[CH:7]2)=[CH:13]1

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 21541252N-formyl-N-methyl-2-phenyl-acetamideHCID 21541268N-methyl-2H-3-isoquinolone sulfate

Produkt 1

HCID 12435498N-methyl-2H-3-isoquinoloneAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 80 g. N-formyl-N-methyl-2-phenyl-acetamide in 200 ml. concentrated sulfuric acid is left to stand for 12 hours at ambient temperature in an atmosphere of nitrogen. This solution is then poured, while stirring, into 1 liter ethanol and cooled in an ice bath in order to maintain the temperature at about 20°-30°C. The crystalline product obtained is filtered off and washed with cold ethanol and dried. There are obtained 70 g. N-methyl-2H-3-isoquinolone sulfate, which has a melting point of 235°-236°C.; yield 60% of theory. The analysis shows that it is a compound of the empirical formula C10H9NO.H2SO4 :

Aufarbeitung

  1. additionThis solution is then poured
  2. temperaturecooled in an ice bath in order
  3. temperatureto maintain the temperature at about 20°-30°C
  4. customThe crystalline product obtained
  5. filtrationis filtered off
  6. washwashed with cold ethanol
  7. customdried
  8. customThere are obtained 70 g

Quellen und Nachweise

ORD-Eintrag
ord-2d7a8a4c651e41c6ae185447404ec26e
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03954771

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