Methanol → HCID 14372494, Verbindung

HRID 1382728Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1382728
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.CO.Cl[C:16]1[N:21]=[CH:20][CH:19]=[CH:18][N:17]=1>C(N(CC)CC)C>[N:17]1[CH:18]=[CH:19][CH:20]=[N:21][C:16]=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 887MethanolHCID 744042-ChloropyrimidineHCID 3082386Quinoline-8-thiol hydrochloride

Produkt 1

HCID 14372494HCID 14372494, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To a solution of 210 mg. (1.06 m mole) of quinoline-8-thiolhydrochloride in 5 ml. of dry methanol was added 128 mg. (1.05 m mole) of 2-chloropyrimidine in 2 ml. of the same solvent followed by 148 ul (1 m mole) 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-5d7bb971accd468f8a0d46d84e762586
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04808591

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