Hydrochloric Acid → 3-(2-Amino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

HRID 1901612Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1901612
CC(O)C.Cl.C(OC([NH:13][CH:14]([CH2:27][O:28][C:29]([NH:31][CH3:32])=[O:30])[CH2:15][O:16][C:17]1[C:21]2[CH:22]=[C:23]([Cl:26])[CH:24]=[CH:25][C:20]=2[O:19][N:18]=1)=O)(C)(C)C>CO>[ClH:26].[NH2:13][CH:14]([CH2:27][O:28][C:29]([NH:31][CH3:32])=[O:30])[CH2:15][O:16][C:17]1[C:21]2[CH:22]=[C:23]([Cl:26])[CH:24]=[CH:25][C:20]=2[O:19][N:18]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 3776Isopropanol2×HCID 23368486HCID 23368486, Verbindung

Produkt 1

HCID 233684343-(2-Amino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

In 10 ml of methanol is dissolved 3-(2-tert-butoxycarbonylamino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole, and to this solution is added 9.6 ml of a 2-propanol solution (7.5N) of hydrogen chloride, and they are subjected to reaction at 20°-25° C. for 4.5 hours. The solvent is removed from the reaction mixture by distillation under reduced pressure, and to the residue obtained is added 5 ml of 2-propanol, after which the crystals precipitated are collected by filtration, to obtain 0.30 g of colorless, crystalline 3-(2-amino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 206°-209° C.

Aufarbeitung

  1. customare subjected to reaction at 20°-25° C. for 4.5 hours
  2. customThe solvent is removed from the reaction mixture by distillation under reduced pressure
  3. customto the residue obtained
  4. customafter which the crystals precipitated
  5. filtrationare collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-303b994a51634e5d92f9986586fbfa76
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05578627

Notizen zur Reaktion

Wird geladen…