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Hydrochloric Acid → HCID 67764133, compound

HRID 439325
Notes
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Reaction equation

HRID 439325 reaction equation
[NH2:1][C:2]1[C:10]([NH2:11])=[CH:9][C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[ClH:13]>O>[ClH:13].[ClH:13].[NH2:1][C:2]1[C:10]([NH2:11])=[CH:9][C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 224111292,3-Diamino-5-fluoro-benzoic acid

Product 1

HCID 67764133HCID 67764133, compoundYield 77%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2,3-diamino-5-fluorobenzoic acid (100 mg, 0.59 mmol) was combined with water (10 mL) in a small reaction vial. To this solution was slowly bubbled hydrogen chloride gas until all the solid dissolved, approximately 30 seconds. The solvents were removed in vacuo to produce a dark solid of 2,3-diamino-5-fluorobenzoic acid dihydrochloride (110 mg, 77%) which was identical in all respects to the sample prepared in Method A.: m.p. 215°-217° (dec); 1H NMR (400 MHz, D2O) δ 7.11 (dd, 1H), 7.43 (dd, 1H); 13C NMR (100 MHzD2O) δ 102.4, 102.7, 104.6, 104.8, 109.3, 109.4, 137.0, 138.5, 138.6, 152.0, 154.8, 170.1.

Workup

  1. dissolutiondissolved, approximately 30 seconds
  2. customThe solvents were removed in vacuo

Sources & evidence

ORD record
ord-9cc6713afe2c42b48beba6d66352dbfa
Source dataset
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05514676

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes