Thiophenol → HCID 19821224, 화합물

HRID 1030204노트

반응식

HRID 1030204 반응식
F[C:2]1[CH:33]=[CH:32][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=3)([F:22])[CH:16]([F:21])[C:17]([F:20])([F:19])[F:18])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:40]1([SH:46])[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>CN(C)C=O>[C:40]1([S:46][C:2]2[CH:3]=[CH:4][C:5]([C:6]([C:8]3[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=4)([F:22])[CH:16]([F:21])[C:17]([F:19])([F:20])[F:18])=[CH:10][CH:9]=3)=[O:7])=[CH:32][CH:33]=2)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1

참가 물질

5

반응물 3

HCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 19821204HCID 19821204, 화합물

생성물 1

HCID 19821224HCID 19821224, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

33 g 4-fluoro-4'-(1-(3-methoxyphenoxy)-1,2,3,3,3-pentafluoro-propoxy)benzophenone, 10 g potassium carbonate, 7.7 g thiophenol, and 100 ml dimethylformamide were stirred together for eight hours at 100° C., then allowed to cool to room temperature. After cooling, the solids were removed from the mixture by filtration, and the low boilers were removed by distillation at 200° C./0.5 mm Hg. The resulting product was distilled at 240°-300° C./0.5 mm Hg. NMR spectra and gas chromatography confirmed that the desired benzophenone was prepared.

후처리

  1. temperatureAfter cooling
  2. customthe solids were removed from the mixture by filtration
  3. customthe low boilers were removed by distillation at 200° C./0.5 mm Hg
  4. distillationThe resulting product was distilled at 240°-300° C./0.5 mm Hg
  5. customwas prepared

출처 및 근거

ORD 기록
ord-5c7f59391f394b18943bc6c57db533ea
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104559

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