Hydrochloric Acid → HCID 178513040, compound

HRID 436903Notes

Reaction equation

HRID 436903 reaction equation
[CH2:1]([NH:9][C:10]([NH:12][C:13]([NH2:15])=[NH:14])=[NH:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.[Na].[Cl:18][CH:19]([Cl:23])[C:20]([OH:22])=[O:21]>C(OCC)(=O)C>[Cl:18][CH:19]([Cl:23])[C:20]([OH:22])=[O:21].[Cl:18][CH:19]([Cl:23])[C:20]([OH:22])=[O:21].[CH2:1]([NH:9][C:10]([NH:12][C:13]([NH2:15])=[NH:14])=[NH:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 6597Dichloroacetic AcidHCID 5360545SodiumHCID 178513039HCID 178513039, compound

Product 1

HCID 178513040HCID 178513040, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

161.0 G. of 1-phenethylbiguanide.HCl, 101.0 g. of sodium dichloroacetae and 216.0 g. of dichloroacetic acid were boiled together in 4.5 l. of absolute ethyl acetate at reflux for 1 hour. The hot solution was filtered under suction in order to separate the precipitated sodium chloride. The filtrate was concentrated in vacuo and treated with diisopropylether, whereby 1-phenethylbiguanide bis-(dichloroacetate) crystallized out analytically pure, M.P.: 131°-132° C.

Workup

  1. filtrationThe hot solution was filtered under suction in order
  2. customto separate the precipitated sodium chloride
  3. concentrationThe filtrate was concentrated in vacuo
  4. additiontreated with diisopropylether, whereby 1-phenethylbiguanide bis-(dichloroacetate)
  5. customcrystallized out analytically pure

Sources & evidence

ORD record
ord-a0e9c9ba2e48447eaad72ff7b939bea6
Source dataset
uspto-grants-1977_06
Patent number
US04028402

Reaction notes

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