Hydrochloric Acid → 3-[2-Amino-3-(4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole dihydrochloride
Reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([NH:38]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:13][C:14]3[N:15]=[CH:16][N:17](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:18]=3)[C:6]=2[CH:58]=1.CC(O)C.[ClH:63]>C(Cl)Cl>[ClH:1].[ClH:63].[NH2:38][CH:12]([CH2:13][C:14]1[N:15]=[CH:16][NH:17][CH:18]=1)[CH2:11][O:10][C:7]1[C:6]2[CH:58]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 0.91 g of 5-chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole in 2 ml of methylene chloride is added 2.2 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 24 hours, after which the solvent is removed by distillation under reduced pressure. Diisopropyl ether is added to the residue obtained and the crystals precipitated are collected by filtration, to obtain 0.4 g of colorless, crystalline 3-[2-amino-3-(4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole dihydrochloride having a melting point of 246.0°-248.4° C. (decomp.).
Workup
- customthey are subjected to reaction at the same temperature for 24 hours
- customafter which the solvent is removed by distillation under reduced pressure
- additionDiisopropyl ether is added to the residue
- customobtained
- customthe crystals precipitated
- filtrationare collected by filtration
Sources & evidence
- ORD record
- ord-8f6dddd39926469f858d4813f83b0121
- Source dataset
- uspto-grants-1996_11
- Patent number
- US05578627
Reaction notes
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