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

HRID 908199ノート

反応式

HRID 908199 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

反応条件

温度
115 °C

実験手順

A stirred mixture of 3-fluoro-4-methanesulfonyl-benzaldehyde (Example 68a) (20 g, 99 mmol), nitroethane (58 ml, 811 mmol) and ammonium acetate (2.29 g, 29 mmol) is heated at reflux (115° C.) under argon for 18 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 is used immediately in the next step.

後処理

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

出典と根拠

ORDレコード
ord-79c54b7011f74a60aaa8f5c454541f0c
出典データセット
uspto-grants-2011_09
特許番号
US08017608B2

反応ノート

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