Hydrochloric Acid → HCID 178479236, compound

HRID 1901654Notes

Reaction equation

HRID 1901654 reaction equation
C(OC([NH:8][CH:9]([CH2:22][C:23]1[O:27][N:26]=[C:25]([OH:28])[CH:24]=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[O:27][N:26]=[C:25]([OH:28])[CH:24]=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 178453744HCID 178453744, compound

Product 1

HCID 178479236HCID 178479236, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 0.38 g of 3-[2-tert-butoxycarbonylamino-3-(3-hydroxy-5-isoxazolyl)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 six hours, after which the solvent is removed by distillation under reduced pressure. Ethyl acetate is added to the residue obtained and the crystals precipitated are collected by filtration, to obtain 0.22 g of pale yellow, crystalline 3-[2-amino-3-(3-hydroxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 188.5°-193.5° C. (decomp.).

Workup

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

Sources & evidence

ORD record
ord-a5e47b0e24c140f2b3f536405ba29e2b
Source dataset
uspto-grants-1996_11
Patent number
US05578627

Reaction notes

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