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

HRID 1901647Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1901647
C(OC([NH:8][CH:9]([CH2:22][C:23]#[N:24])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=O)(C)(C)C.CC(O)C.Cl.C(OC(C)C)(C)C>CO>[ClH:21].[NH2:8][CH:9]([CH2:22][C:23]#[N:24])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 7914Diisopropyl EtherHCID 233685283-(2-Tert-butoxycarbonylamino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole

Produkt 1

HCID 233684313-(2-Amino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a suspension of 1.0 g of 3-(2-tert-butoxycarbonylamino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole in 15 ml of methanol is added 7.8 ml of a 2-propanol solution (6.5M) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for seven hours. Thereafter, the solvent is removed by distillation under reduced pressure. To the residue obtained is added diisopropyl ether, and the crystals precipitated are collected by filtration, to obtain 0.78 g of colorless, crystalline 3-(2-amino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 188.8°-190.9° C. (decomp.).

Aufarbeitung

  1. customthey are subjected to reaction at the same temperature for seven hours
  2. customThereafter, 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-1c4d6d544f1e4798b912a69b9d8488f1
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05578627

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