Hydrochloric Acid → HCID 23368544, compound

HRID 1901644Notes

Reaction equation

HRID 1901644 reaction equation
C(OC([NH:8][CH:9]([CH2:22][C:23]1[N:24]=[CH:25][N:26]([C:28](=[O:32])[N:29]([CH3:31])[CH3:30])[CH:27]=1)[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>CO>[ClH:21].[NH2:8][CH:9]([CH2:22][C:23]1[N:24]=[CH:25][N:26]([C:28](=[O:32])[N:29]([CH3:31])[CH3:30])[CH:27]=1)[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

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 23368508HCID 23368508, compound

Product 1

HCID 23368544HCID 23368544, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 0.2 g of 3-[2-tert-butoxycarbonylamino-3-(1-dimethylcarbamoyl-4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole in 2 ml of methanol is added 1.2 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 ten 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 0.1 g of pale brown, crystalline 3-[2-amino-3-(1-dimethylcarbamoyl-4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 167.0°-169.5° C. (decomp.).

Workup

  1. customthey are subjected to reaction at the same temperature for ten hours
  2. customafter which the solvent is removed by distillation under reduced pressure
  3. additionDiisopropyl ether is added to the residue
  4. customobtained
  5. customthe crystals precipitated
  6. filtrationare collected by filtration

Sources & evidence

ORD record
ord-79f43f34fb0948ee95d97b7ee25684f7
Source dataset
uspto-grants-1996_11
Patent number
US05578627

Reaction notes

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