Hydrochloric Acid → HCID 23368565, compound

HRID 1901658Notes

Reaction equation

HRID 1901658 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:19]C(OC(C)(C)C)=O)[CH2:13][O:14][S:15](=[O:18])(=[O:17])[NH2:16])[C:6]=2[CH:27]=1.O1CCOCC1.Cl.C(OCC)(=O)C>CO>[ClH:1].[NH2:19][CH:12]([CH2:13][O:14][S:15](=[O:17])(=[O:18])[NH2:16])[CH2:11][O:10][C:7]1[C:6]2[CH:27]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 312751,4-DioxaneHCID 23368380HCID 23368380, compound

Product 1

HCID 23368565HCID 23368565, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 0.4 g of 5-chloro-3-(2-tert-butoxycarbonylamino-3-sulfamoyloxypropoxy)-1,2-benzoisoxazole in 10 ml of methanol is added 5 ml of a dioxane solution (3.2N) 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. To the residue obtained is added 10 ml of ethyl acetate, and the crystals precipitated are collected by filtration, to obtain 0.24 g of colorless, crystalline 3-(2-amino-3-sulfamoyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 150.5°-152.5° C. (decomp.).

Workup

  1. customthey are subjected to reaction at the same temperature for 24 hours
  2. customafter which the solvent is removed by distillation under reduced pressure
  3. customTo the residue obtained
  4. customthe crystals precipitated
  5. filtrationare collected by filtration

Sources & evidence

ORD record
ord-feaf4a4bf1df433da425395ef971eb2b
Source dataset
uspto-grants-1996_11
Patent number
US05578627

Reaction notes

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