HCID 4372276, compound → HCID 131710394, compound

HRID 918105Notes

Reaction equation

HRID 918105 reaction equation
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6]1([CH3:18])[O:10][C:9]2[CH:11]=[CH:12][C:13]([N+:15]([O-])=O)=[CH:14][C:8]=2[O:7]1)[CH3:2].[H][H]>[Ni]>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6]1([CH3:18])[O:10][C:9]2[CH:11]=[CH:12][C:13]([NH2:15])=[CH:14][C:8]=2[O:7]1)[CH3:2]

Participants

4

Reactant 2

HCID 4372276HCID 4372276, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 131710394HCID 131710394, compound

Reagents, catalysts & solvents 1

HCID 935NickelCatalyst

Procedure

of ethyl(2-methyl-5-nitro-1,3-benzodioxol-2-yl)-acetate (prepared according to G. Sloof, Rec. Trav. Chim. 547, 995 (1935)) dissolved in 300 cc. of 95% alcohol are hydrogenated at room temperature and 2 atm. of hydrogen pressure in the presence of 6 g. of Raney nickel. After the theoretical absorption of hydrogen, the mixture is filtered and evaporated to dryness. The residual oil is purified by distillation, (b.p. 190°-200°C./0.4 mm.).

Workup

  1. customare hydrogenated at room temperature
  2. customAfter the theoretical absorption of hydrogen
  3. filtrationthe mixture is filtered
  4. customevaporated to dryness
  5. distillationThe residual oil is purified by distillation, (b.p. 190°-200°C./0.4 mm.)

Sources & evidence

ORD record
ord-7af12781928f4fb896fb6b08c56a6d00
Source dataset
uspto-grants-1976_07
Patent number
US03969368

Reaction notes

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