Hydrochloric Acid → HCID 20131352, compound

HRID 1789062Notes

Reaction equation

HRID 1789062 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% palladium-on-carbon in a circulating 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, 2-propanol and ether are added, and 35 g (97%) of 2,2-difluoro-1,3-benzodioxole-4,5-diamine dihydrochloride of m.p. 232°-233° C. (decomposition) are obtained.

Workup

  1. filtrationthe mixture is filtered
  2. concentrationthe solution is concentrated in vacuo, 2-propanol and ether
  3. additionare added

Sources & evidence

ORD record
ord-afc1b28b948743f0ab162dbe3eb3f56e
Source dataset
uspto-grants-1987_08
Patent number
US04686230

Reaction notes

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