Sodium Methoxide → HCID 3357995, compound

HRID 1903158Notes

Reaction equation

HRID 1903158 reaction equation
[CH3:1][C:2]1([CH3:18])[O:6][C:5]2[CH:7]=[C:8]([N+:15]([O-:17])=[O:16])[C:9]([NH:11]C(C)=O)=[CH:10][C:4]=2[O:3]1.C[O-].[Na+]>CO>[CH3:1][C:2]1([CH3:18])[O:6][C:5]2[CH:7]=[C:8]([N+:15]([O-:17])=[O:16])[C:9]([NH2:11])=[CH:10][C:4]=2[O:3]1

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 13343746HCID 13343746, compound

Product 1

HCID 3357995HCID 3357995, compoundYield 92.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

22.0 g of 2,2-dimethyl-5-acetamino-6-nitro-1,3-benzodioxole were boiled under reflux for 1 hour in 1.1 l of methanol containing 2.2 g of sodium methoxide (10% by weight). After evaporating the solution, the residue was dissolved in methylene chloride, filtered first through Decalit and then through silicon dioxide evaporated and crystallized from isopropanol. There were obtained 17.0 g (92.8% of theory) of 2,2-dimethyl-5-amino-6-nitro-1,3-benzodioxole of melting point 128°-129° C.

Workup

  1. customAfter evaporating the solution
  2. dissolutionthe residue was dissolved in methylene chloride
  3. filtrationfiltered first through Decalit
  4. customthrough silicon dioxide evaporated
  5. customcrystallized from isopropanol

Sources & evidence

ORD record
ord-800c5be65c6946f489543231674679b5
Source dataset
uspto-grants-1984_03
Patent number
US04435406

Reaction notes

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