2,4'-Dichloroacetophenone → 2-(4-Chlorophenyl)-2-oxoethyl thiocyanate

HRID 604874

反応式

HRID 604874 の反応式
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1)=[O:4].[C:12]([S-:14])#[N:13].[K+]>>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([C:3](=[O:4])[CH2:2][S:14][C:12]#[N:13])=[CH:6][CH:7]=1

参加物

3

反応物 2

HCID 702982,4'-DichloroacetophenoneHCID 516872Potassium thiocyanate

生成物 1

HCID 880132-(4-Chlorophenyl)-2-oxoethyl thiocyanate収率 90%

実験手順

A solution of 945 mg (5 mmol) 2,4′-dichloroacetophenone and 583 mg (6 mmol) potassium rhodanide was heated to reflux for 30 minutes. After a few minutes a precipitation was formed. The solvent was evaporated under reduced pressure and the residue was suspended in tetrahydrofurane, stirred for 1 hour at room temperature, filtered and the filtrate was concentrated in vacuo. The residue was stirred with heptane and little ethanol for 15 minutes. The product was filtered off and dried to yield 953 mg (90%) 1-(4-chloro-phenyl)-2-thiocyanato-ethanone as a light yellow solid. 1H NMR (CDCl3, 250 MHz): δ (ppm)=7.89 (d, 2H), 7.51 (d, 2H), 4.692 (s, 2H).

後処理

  1. temperatureto reflux for 30 minutes
  2. customAfter a few minutes a precipitation
  3. customwas formed
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated in vacuo
  7. stirringThe residue was stirred with heptane and little ethanol for 15 minutes
  8. filtrationThe product was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-f236601bf5e449eeadf020241375a1af
出典データセット
uspto-grants-2011_03
特許番号
US07910740B2

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