Benzene → HCID 70216990, compound

HRID 2269775Notes

Reaction equation

HRID 2269775 reaction equation
[CH:1]1C=CC=CC=1.[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([N+:16]([O-:18])=[O:17])=[C:12]([CH:15]=1)[CH:13]=O.CCCCCC.[C:25]([O:28][CH2:29][CH3:30])(=[O:27])[CH3:26]>>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([N+:16]([O-:18])=[O:17])=[C:12]([CH:13]=[C:26]([CH3:1])[C:25]([O:28][CH2:29][CH3:30])=[O:27])[CH:15]=1

Participants

4

Reactant 3

HCID 241BenzeneHCID 811235-Chloro-2-nitrobenzaldehydeHCID 21226206Ethyl acetate hexane

Product 1

HCID 70216990HCID 70216990, compound

Procedure

To 200 ml of benzene, 10.0 g (53.8 mmol) of 5-chloro-2-nitrobenzaldehyde (manufactured by Aldrich Chemical Co., Inc.) and 18.1 g (50.0 mmol) of Wittig reagent (carbethoxyethylidene triphenylphosphorane, manufactured by Aldrich Chemical Co., Inc.) were added, and the mixture m was stirred at room temperature for one night. After the completion of the reaction was verified by TLC, the reaction liquid was concentrated, whereby a crude product was obtained. This crude product was refined by a column chromatography (aminopropyl-modified silica gel (Fuji Silysia Chem. Co., NH-DM); developing agent: hexane/ethyl acetate=1/1), whereby 13.3 g of the aimed compound were obtained as a crystal (yield: 98%).

Workup

  1. customthe reaction liquid
  2. concentrationwas concentrated
  3. customwhereby a crude product was obtained

Sources & evidence

ORD record
ord-5b0dc7749ac942caafd67b8da4378611
Source dataset
uspto-grants-2001_12
Patent number
US06329546B1

Reaction notes

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