Sodium Carbonate → HCID 13537214, Verbindung

HRID 235653

Reaktionsgleichung

Reaktionsgleichung von HRID 235653
[NH2:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][CH3:9])[CH2:3]1.C(=O)([O-])[O-].[Na+].[Na+].Cl.[Cl:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22]([NH:28][C:29]3[CH:34]=[CH:33][C:32]([S:35](Cl)(=[O:37])=[O:36])=[CH:31][CH:30]=3)=[CH:23][N:24]=[N:25]2)=[CH:20][CH:19]=1>C(Cl)(Cl)Cl.O>[Cl:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22]([NH:28][C:29]3[CH:30]=[CH:31][C:32]([S:35]([NH:1][CH:2]4[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][CH3:9])[CH2:3]4)(=[O:36])=[O:37])=[CH:33][CH:34]=3)=[CH:23][N:24]=[N:25]2)=[CH:20][CH:19]=1

Komponenten

6

Edukt 3

HCID 10340Sodium CarbonateHCID 980943-amino-N-ethylpiperidineHCID 21273956HCID 21273956, Verbindung

Produkt 1

HCID 13537214HCID 13537214, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
3 °C

Versuchsvorschrift

3-Amino-1-ethylpiperidine (0.4 ml) in chloroform (15 ml) was treated with anhydrous sodium carbonate (2.94 g) in water (15 ml) and cooled to 3° C. The mixture was vigorously stirred and treated with 4-(7-chloro-4-cinnolinylamino)benzenesulphonylchloride hydrochloride (1.0 g). The dark orange mixture was stirred at 3° C. for 15 minutes, then at room temperature for 45 minutes. During this period the colour lightened considerably. The chloroform layer was separated and dried over magnesium sulphate. The residue on evaporation solidified when triturated with methanol, to give the title compound (0.5 g), m.p. 213°-15° C. (with decomposition).

Aufarbeitung

  1. stirringThe dark orange mixture was stirred at 3° C. for 15 minutes
  2. waitDuring this period the colour lightened considerably
  3. customThe chloroform layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customThe residue on evaporation
  6. customtriturated with methanol

Quellen und Nachweise

ORD-Eintrag
ord-f64cd5b988b14d4f8e6425d0bb08320b
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04640920

Verknüpfte Notizen

Wird geladen…