Water → 2-Tert-butyl-5-(4-methylpiperidin-1-yl)-6-nitrobenzothiazole

HRID 5785

Reaktionsgleichung

Reaktionsgleichung von HRID 5785
[C:1]([C:5]1[S:6][C:7]2[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11](Cl)=[CH:10][C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:18][CH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O.C(Cl)(Cl)Cl>[C:1]([C:5]1[S:6][C:7]2[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11]([N:22]3[CH2:23][CH2:24][CH:19]([CH3:18])[CH2:20][CH2:21]3)=[CH:10][C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

7

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 693814-MethylpiperidineHCID 197942022-Tert-butyl-5-chloro-6-nitrobenzothiazole

Produkt 1

HCID 197941892-Tert-butyl-5-(4-methylpiperidin-1-yl)-6-nitrobenzothiazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A solution of 32,4 g of 2-tert-butyl-5-chloro-6-nitrobenzothiazole, (described in European patent application 85810418.5 published under No. 0175650) in 300 ml of dimethylsulphoxide, is stirred and heated at 140° for 6 hours with 12.8 g of 4-methylpiperidine and 35.8 g of anhydrous potassium carbonate, cooled and poured into water. The solid obtained is dissolved in chloroform and filtered through a silical gel column. The filtate is evaporated to give 2-tert-butyl-5-(4-methylpiperidin-1-yl)-6-nitrobenzothiazole melting at 116°-120°.

Aufarbeitung

  1. temperaturecooled
  2. customThe solid obtained
  3. filtrationfiltered through a silical gel column
  4. customThe filtate is evaporated

Quellen und Nachweise

ORD-Eintrag
ord-269df9c1e534472b9cb72738c8208fee
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05246927

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