Potassio isocyanate → N-(4,4-Dimethyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-7-yl)urea

HRID 621416

Reaktionsgleichung

Reaktionsgleichung von HRID 621416
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:15])([CH3:14])[C:7](=[O:13])[NH:8][C:9]2=[O:12])=[CH:4][CH:3]=1.[N-:16]=[C:17]=[O:18].[K+]>C(O)(=O)C>[CH3:14][C:6]1([CH3:15])[C:5]2[C:10](=[CH:11][C:2]([NH:1][C:17]([NH2:16])=[O:18])=[CH:3][CH:4]=2)[C:9](=[O:12])[NH:8][C:7]1=[O:13]

Komponenten

4

Edukt 2

HCID 11051572Potassio isocyanateHCID 135581517-amino-4,4-dimethylisoquinoline-1,3(2H,4H)-dione

Produkt 1

HCID 21242858N-(4,4-Dimethyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-7-yl)urea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

1.3 g. (6.3 mMole) 7-amino-4,4-dimethylisoquinoline-1,3-dione was suspended in 30 ml. 2N acetic acid, mixed with 1.0 g. (12.5 mMole) potassium isocyanate and stirred for 6 hours at 80° C. The reaction mixture was cooled and the precipitate was filtered off with suction and washed with water. The residue was dissolved in dilute aqueous sodium hydroxide solution, the solution was neutralised with dilute hydrochloric acid, the residue was filtered off with suction and, for purification, worked up with ethanol and filtered off with suction. Yield: 0.6 g. (38.5% of theory); m.p. 260°-264° C.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. filtrationthe precipitate was filtered off with suction
  3. washwashed with water
  4. dissolutionThe residue was dissolved in dilute aqueous sodium hydroxide solution
  5. filtrationthe residue was filtered off with suction and, for purification
  6. filtrationfiltered off with suction

Quellen und Nachweise

ORD-Eintrag
ord-e606f20b4a8b483aa06baaab95ff68a3
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04824835

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