Ethanol → HCID 23454854, compound

HRID 1680875Notes

Reaction equation

HRID 1680875 reaction equation
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH:10](Cl)[C:11]([CH3:16])([N+:13]([O-:15])=[O:14])[CH3:12])=[CH:4][C:3]=2[O:2]1.Cl(O)(=O)(=O)=O.C(O)C>[H][H].C(OCC)(=O)C.[C].[Pd]>[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11]([CH3:16])([N+:13]([O-:15])=[O:14])[CH3:12])=[CH:4][C:3]=2[O:2]1

Participants

7

Reactant 3

HCID 702EthanolHCID 24247Perchloric AcidHCID 234548395-(1-Chloro-2-methyl-2-nitropropyl)-2H-1,3-benzodioxole

Product 1

HCID 23454854HCID 23454854, compoundYield 89%

Reagents, catalysts & solvents 3

HCID 178418390HCID 178418390, compoundCatalystHCID 8857Ethyl AcetateSolventHCID 178418361HCID 178418361, compoundSolvent

Procedure

A mixture of 7.0 g of 1-(3,4-methylenedioxyphenyl)-1-chloro-2-methyl-2-nitropropane, 7.7 g of 70% perchloric acid, 2.8 g of 10% palladium-carbon and 100 ml of ethanol is shaken at room temperature for 3 hours in hydrogen gas atmosphere under 3 atmospheres. After the reaction, insoluble materials are removed by filtration, and the filtrate is condensed. The residue is dissolved in ethyl acetate, and the solution is washed with water, a saturated sodium bicarbonate solution and a saturated sodium chloride solution, successively. The washed solution is dried and then evaporated to remove solvent. 5.4 g of 1-(3,4-methylenedioxyphenyl)-2-methyl-2-nitropropane are thereby obtained as an oil.

Workup

  1. customAfter the reaction, insoluble materials
  2. customare removed by filtration
  3. customcondensed
  4. washthe solution is washed with water
  5. customThe washed solution is dried
  6. customevaporated
  7. customto remove solvent

Sources & evidence

ORD record
ord-bfac1b3d2d884b7dbc198abab3a85a5f
Source dataset
uspto-grants-1981_06
Patent number
US04276304

Reaction notes

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