Hydrochloric Acid → HCID 20131352, compound

HRID 638232Notes

Reaction equation

HRID 638232 reaction equation
[NH2:1][C:2]1[C:10]2[O:9][C:8]([F:12])([F:11])[O:7][C:6]=2[CH:5]=[CH:4][C:3]=1[N+:13]([O-])=O.[ClH:16]>CO.[Pd]>[ClH:16].[ClH:16].[F:12][C:8]1([F:11])[O:7][C:6]2=[CH:5][CH:4]=[C:3]([NH2:13])[C:2]([NH2:1])=[C:10]2[O:9]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 20131417HCID 20131417, compound

Product 1

HCID 20131352HCID 20131352, compoundYield 97%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

30 g of 4-amino-2,2-difluoro-5-nitro-1,3-benzodioxole are hydrogenated in 300 ml of methanol on 0.5 g of 10% strength palladium-on-charcoal in a circulatory hydrogenation apparatus under atmospheric pressure and at room temperature, 2.5 equivalents of methanolic hydrogen chloride solution are added, the mixture is filtered, the solution is concentrated in vacuo and isopropanol and ether are added to the residue to give 35 g (97%) of 2,2-difluoro-1,3-benzodioxole-4,5-diamine dihydrochloride of m.p. 232°-233° C. (decomposition).

Workup

  1. filtrationthe mixture is filtered
  2. concentrationthe solution is concentrated in vacuo and isopropanol and ether
  3. additionare added to the residue

Sources & evidence

ORD record
ord-7a0d98996d4d43e2b38ad75a5b230dc9
Source dataset
uspto-grants-1985_12
Patent number
US04560693

Reaction notes

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