Acetonitrile → 3-(2,4-Dichlorophenyl)-3-oxopropanenitrile

HRID 732947

反応式

HRID 732947 の反応式
[C:1](#[N:3])[CH3:2].[Li]CCCC.[Cl:9][C:10]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:11]=1[C:12](Cl)=[O:13]>C1COCC1>[Cl:9][C:10]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:11]=1[C:12](=[O:13])[CH2:2][C:1]#[N:3]

参加物

5

実験手順

To a stirred solution of acetonitrile (2.0 mL, 38.2 mmol) in THF (50 mL) at −78° C. was added nBuLi (1.81 M in hexane, 16 mL, 28.7 mmol). The resulting slurry was kept at −78° C. for 15 min and 2,4-dichlorobenzoyl chloride (2.0 g, 9.55 mmol) was added dropwise to the acetonitrile anion. After 40 min, the reaction was quenched by addition of saturated NH4Cl (30 mL). THF was removed under reduced pressure and the suspension was filtered. The solid was washed with H2O (100 mL) and dried to give 3-(2,4-dichlorophenyl)-3-oxopropanenitrile (2.0 g, 98%, >95% purity) as a light yellow solid.

後処理

  1. waitAfter 40 min
  2. customthe reaction was quenched by addition of saturated NH4Cl (30 mL)
  3. customTHF was removed under reduced pressure
  4. filtrationthe suspension was filtered
  5. washThe solid was washed with H2O (100 mL)
  6. customdried

出典と根拠

ORDレコード
ord-944f8150ba9f49919021ddc8a8e53b70
出典データセット
uspto-grants-2009_09
特許番号
US07589088B2

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