Benzene → HCID 70216990, compound

HRID 1976893Notes

Reaction equation

HRID 1976893 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 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-9a4ca84a0eaa4fc0b4b1d63c00399915
Source dataset
uspto-grants-2001_05
Patent number
US06229020B1

Reaction notes

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