Triethylamine → HCID 14372494, Verbindung

HRID 1723024Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1723024
Cl.[N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[SH:12])[CH:5]=[CH:4][CH:3]=1.Cl[C:14]1[N:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C(N(CC)CC)C>CO>[N:15]1[CH:16]=[CH:17][CH:18]=[N:19][C:14]=1[S:12][C:10]1[CH:9]=[CH:8][CH:7]=[C:6]2[C:11]=1[N:2]=[CH:3][CH:4]=[CH:5]2

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 744042-ChloropyrimidineHCID 3082386Quinoline-8-thiol hydrochloride

Produkt 1

HCID 14372494HCID 14372494, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 210 mg. (1.06 m mole) of quinoline-8-thiol hydrochloride in 5 ml. of dry methanol was added 128 mg. (1.05 mmol) of 2-chloropyrimidine in 2 ml. of the same solvent followed by 0.148 ml (1 mmol) of dry triethylamine. The reaction mixture was allowed to stir at room temperature overnight followed by the removal of the methanol in vacuo. The residue was partitioned between a saturated sodium bicarbonate solution and ethyl acetate. The organic phase was separated, dried and concentrated. The residue was redissolved in chloroform and concentrated without heat. The residue was triturated with ethyl acetate, filtered and dried, 170 mg., m.p. 165°-168° C.

Aufarbeitung

  1. customfollowed by the removal of the methanol in vacuo
  2. customThe residue was partitioned between a saturated sodium bicarbonate solution and ethyl acetate
  3. customThe organic phase was separated
  4. customdried
  5. concentrationconcentrated
  6. dissolutionThe residue was redissolved in chloroform
  7. concentrationconcentrated
  8. temperaturewithout heat
  9. customThe residue was triturated with ethyl acetate
  10. filtrationfiltered
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-39115f5f66bf4fc7873ac3dea8bc284f
Quelldatensatz
uspto-grants-1989_08
Patentnummer
US04859679

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