Hydrochloric Acid → HCID 67733454, compound

HRID 1901637Notes

Reaction equation

HRID 1901637 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][C@@H:12]([NH:16]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:13][S:14][CH3:15])[C:6]=2[CH:36]=1.CC(O)C.Cl>CO>[ClH:1].[NH2:16][C@@H:12]([CH2:13][S:14][CH3:15])[CH2:11][O:10][C:7]1[C:6]2[CH:36]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 67733418HCID 67733418, compound

Product 1

HCID 67733454HCID 67733454, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 2.41 g of (R)-5-chloro-3-(3-methylthio-2-tritylaminopropoxy)-1,2-benzoisoxazole in 5 ml of methanol is added 6.0 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 three 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 and dried, to obtain 0.72 g of colorless, crystalline (R)-3-(2-amino-3-methylthiopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 195.0°-198.2° C. (decomp.).

Workup

  1. customthey are subjected to reaction at the same temperature for three 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
  7. customdried

Sources & evidence

ORD record
ord-a3f1eda3363e407a83ef7525558c9ef8
Source dataset
uspto-grants-1996_11
Patent number
US05578627

Reaction notes

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