Acetic Acid Mixture with Hydrobromic Acid → HCID 20247127, compound

HRID 1981414Notes

Reaction equation

HRID 1981414 reaction equation
Br.C(O)(=O)C.CS(O)(=O)=O.C(OC([NH:21][CH2:22][CH2:23][C:24]([O:26][C:27]1[CH:32]=[CH:31][C:30]([C:33](=[NH:35])[NH2:34])=[CH:29][C:28]=1[C:36](=[O:43])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)=[O:25])=O)C1C=CC=CC=1>C(OCC)C>[NH2:21][CH2:22][CH2:23][C:24]([O:26][C:27]1[CH:32]=[CH:31][C:30]([C:33](=[NH:34])[NH2:35])=[CH:29][C:28]=1[C:36](=[O:43])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)=[O:25]

Participants

4

Reactant 2

HCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 86740067HCID 86740067, compound

Product 1

HCID 20247127HCID 20247127, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To 4.0 ml of a 30% hydrogen bromide-acetic acid mixture, was added 1.0 g of 4-amidino-2-benzoylphenyl 3-benzyloxycarbonylaminopropionate methanesulfonate. The mixture was stirred for one hour at room temperature to dissolve the crystals, forming a homogeneous yellow solution. Anhydrous ethyl ether was added to the solution to precipitate a white or pale yellow powder. After removing the supernatant, the residue was washed a few times with ethyl ether to obtain 0.5 g of a hydroscopic powder of 4-amidino-2-benzoylphenyl 3-aminopropionate dihydrobromide.

Workup

  1. dissolutionto dissolve the crystals
  2. customforming a homogeneous yellow solution
  3. customto precipitate a white or pale yellow powder
  4. customAfter removing the supernatant
  5. washthe residue was washed a few times with ethyl ether

Sources & evidence

ORD record
ord-6808411c03dc4c12ad9cdc2660663ecf
Source dataset
uspto-grants-1985_04
Patent number
US04514416

Reaction notes

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