Methanesulfonic Acid → 2-(4-Aminophenyl)benzothiazole methanesulphonic acid salt

HRID 363303

Reaktionsgleichung

Reaktionsgleichung von HRID 363303
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][CH:3]=1.[CH3:17][S:18]([OH:21])(=[O:20])=[O:19]>C(OCC)(=O)C>[CH3:17][S:18]([OH:21])(=[O:20])=[O:19].[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 2344752-(4-Aminophenyl)benzothiazole

Produkt 1

HCID 877273232-(4-Aminophenyl)benzothiazole methanesulphonic acid saltAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 2-(4-aminophenyl)benzothiazole (0.5 g, 2.21 mmol) in ethyl acetate (65 ml) was added dropwise methanesulphonic acid (0.215 g, 2.21 mmol) at room temperature. The reaction mixture was stirred for 30 minutes. The product was collected and washed with hot ethyl acetate to give a pale yellow powder (0.67 g, 94%), m.p. 261°-262° C.; vmax /cm-1 3422, 2880, 2633, 1598, 1487, 1322, 1220, 1149, 1043, 967, 780, 755, 561; δH (DMSO-d6) 8.10(1H, d, J7.9, 4-H), 8.00(3H, m, 7, 2', 6'-H), 7.52(1H, t, J7.3, 5-H), 7.42(1H, t, J7.5, 6-H), 7.06(2H, d, J8.5, 3', 5'-H), 5.72(3H, br s, NH3+), 2.41(3H, s, CH3).

Aufarbeitung

  1. customThe product was collected
  2. washwashed with hot ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-5c0dc69af73046c59c49b435471033a0
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05874431

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