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1,2-Ethanediamine, N1,N2-bis(phenylmethyl)-, acetate (1:2) → Benzathine

HRID 1702134
Notes
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Reaction equation

HRID 1702134 reaction equation
C(O)(=O)C.C(O)(=O)C.[CH2:9]([NH:16][CH2:17][CH2:18][NH:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>O>[CH2:9]([NH:16][CH2:17][CH2:18][NH:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 312281,2-Ethanediamine, N1,N2-bis(phenylmethyl)-, acetate (1:2)

Product 1

HCID 8793Benzathine

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

306 mg. (0.001 ml) of BL-P2013 was dissolved in 7 ml. H2O and added to a solution of 180 mg. (0.0005 mol) of N,N'-dibenzylethylenediamine diacetate in 7 ml. H2O. The mixture was stirred and the salt crystallized and after stirring approximately 10-15 minutes the salt was collected by filtration and air dried to yield N,N'-dibenzylethylenediamine salt of BL-P2013 (300 mg). The material was recrystallized by dissolving it in approximately 10 ml. of boiling acetone and diluting with ether to the cloud point. 260 mg. of air dried and vacuum dried material was obtained.

Workup

  1. custom
the salt crystallized
  • stirringafter stirring approximately 10-15 minutes the salt
  • filtrationwas collected by filtration and air
  • customdried
  • Sources & evidence

    ORD record
    ord-8d64be62cfc6453395d567d2b2858ff6
    Source dataset
    uspto-grants-1983_04
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US04380512

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes