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

HRID 604874

반응식

HRID 604874 반응식
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

참가 물질

3

반응물 2

HCID 702982,4'-DichloroacetophenoneHCID 516872Potassium thiocyanate

생성물 1

HCID 880132-(4-Chlorophenyl)-2-oxoethyl thiocyanate수율 90%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f236601bf5e449eeadf020241375a1af
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910740B2

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