Hydrochloric Acid → 5-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride

HRID 1901629Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1901629
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([C:33]3[S:37][C:36]([CH3:38])=[N:35][CH:34]=3)[NH:13]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[C:6]=2[CH:39]=1.CC(O)C.Cl>C(Cl)(Cl)Cl.CO>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([C:33]3[S:37][C:36]([CH3:38])=[N:35][CH:34]=3)[NH2:13])[C:6]=2[CH:39]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 3776Isopropanol2×HCID 233685165-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethoxy]-1,2-benzoisoxazole

Produkt 1

HCID 233685375-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of 1.7 g of 5-chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethoxy]-1,2-benzoisoxazole in 17 ml of chloroform and 17 ml of methanol is added 2.05 ml of a 2-propanol solution (7.5N) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for two hours, after which the solvent is removed by distillation under reduced pressure. To the residue obtained is added 2-propanol, and after stirring, the crystals precipitated are collected by filtration, to obtain 0.90 g of colorless, crystalline 5-chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride having a melting point of 212° C.

Aufarbeitung

  1. customthey are subjected to reaction at the same temperature for two hours
  2. customafter which the solvent is removed by distillation under reduced pressure
  3. customTo the residue obtained
  4. customthe crystals precipitated
  5. filtrationare collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-718cfeffa83a4723b3c85a6fc47989c7
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05578627

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