Ethanol → ethyl 2-chloro-5-nitrobenzoate

HRID 2116549ノート

反応式

HRID 2116549 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].C([O-])([O-])=O.[K+].[K+].[CH2:20](O)[CH3:21]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([O:6][CH2:20][CH3:21])=[O:5]

参加物

5

反応物 3

HCID 702EthanolHCID 11430Potassium CarbonateHCID 172872-Chloro-5-nitrobenzoic acid

生成物 1

HCID 2774222ethyl 2-chloro-5-nitrobenzoate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 2-chloro-5-nitrobenzoic acid (26 g) in ethanol (260 mL) and concentrated sulfuric acid (1 mL) was heated at reflux for 18 hr. The reaction mixture was cooled and K2CO3 was added to quench the reaction. The resulting mixture was filtered and concentrated. The residue was then suspended in ether and filtered to remove insoluble starting acid. The filtrate was washed with 4% KOH (110 mL), dried over MgSO4 and concentrated to provide 16.2 g of ethyl 2-chloro-5-nitrobenzoate as a colorless oil which solidified on standing.

後処理

  1. temperatureat reflux for 18 hr
  2. temperatureThe reaction mixture was cooled
  3. customto quench
  4. customthe reaction
  5. filtrationThe resulting mixture was filtered
  6. concentrationconcentrated
  7. filtrationfiltered
  8. customto remove insoluble
  9. washThe filtrate was washed with 4% KOH (110 mL)
  10. dry with materialdried over MgSO4
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-319b96eb17f84477a76ee7226ae0e324
出典データセット
uspto-grants-2008_10
特許番号
US07439242B2

反応ノート

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