Nitroethane → 2-Fluoro-1-methanesulfonyl-4-(2-nitro-propenyl)-benzene

HRID 1092967ノート

反応式

HRID 1092967 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[S:10]([CH3:13])(=[O:12])=[O:11])[CH:5]=O.[N+:14]([CH2:17][CH3:18])([O-:16])=[O:15].C([O-])(=O)C.[NH4+]>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([CH:5]=[C:17]([N+:14]([O-:16])=[O:15])[CH3:18])[CH:7]=[CH:8][C:9]=1[S:10]([CH3:13])(=[O:12])=[O:11]

参加物

5

反応物 3

HCID 6587NitroethaneHCID 517165Ammonium AcetateHCID 212517323-Fluoro-4-methanesulfonylbenzaldehyde

生成物 1

HCID 665884842-Fluoro-1-methanesulfonyl-4-(2-nitro-propenyl)-benzene

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A stirred mixture of 3-fluoro-4-methanesulfonyl-benzaldehyde (Example 64a) (24 g, 0.119 mol), nitroethane (70 ml, 0.97 mol) and ammonium acetate (2.75 g, 35 mmol) is heated at reflux under argon for 24 hours. The mixture is concentrated to give an oil which is dissolved in chloroform (200 ml) and washed with water (2×200 ml), followed by brine (100 ml). The organic extract is dried (MgSO4), filtered and the solvent removed to give the product as an orange oil. This was used immediately in the next step.

後処理

  1. temperatureis heated
  2. temperatureat reflux under argon for 24 hours
  3. concentrationThe mixture is concentrated
  4. customto give an oil which
  5. washwashed with water (2×200 ml)
  6. extractionThe organic extract
  7. dry with materialis dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent removed

出典と根拠

ORDレコード
ord-ec3d2cb9ce6a41dda4b8182114ebff86
出典データセット
uspto-grants-2012_03
特許番号
US08129541B2

反応ノート

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