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Benzene → 2-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane

HRID 1194770
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HRID 1194770 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)(O)[CH:9]2[S:14][CH2:13][S:12][CH2:11][S:10]2)=[CH:4][CH:3]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>C1CCCCC1>[F:22][C:19]1[CH:20]=[CH:21][C:16]([C:8](=[C:9]2[S:10][CH2:11][S:12][CH2:13][S:14]2)[C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 143292582-{Bis(4-fluorophenyl)hydroxymethyl}-1,3,5-trithiane

생성물 1

HCID 143292842-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane수율 89.5%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

A mixture of 2.0 g of 2-{bis(4-fluorophenyl)hydroxymetyl}-1,3,5-trithiane, 0.2 g of p-toluenesulfonic acid and 50 ml of benzene was refluxed with heating for 15 minutes by means of a Dean-Stark reflux condenser. After being cooled, the mixture was extracted with ethyl acetate and the extract was washed with a saturated aqueous sodium hydrogencarbonate solution. The washed extract was dried over anhydrous magnesium sulfate and the solvent was removed by distillation under reduced pressure to obtain a material, which was recrysallized from cyclohexane to give 1.7 g of the desired compound.

후처리

  1. temperaturewas refluxed
  2. temperaturewith heating for 15 minutes by means of a Dean-Stark
  3. temperaturereflux condenser
  4. temperatureAfter being cooled
  5. extractionthe mixture was extracted with ethyl acetate
  6. washthe extract was washed with a saturated aqueous sodium hydrogencarbonate solution
  7. extractionThe washed extract
  8. dry with materialwas dried over anhydrous magnesium sulfate
  9. customthe solvent was removed by distillation under reduced pressure
  10. customto obtain a material, which

출처 및 근거

ORD 기록
ord-0f0bcebbd6df4aafbc84d24ac2015dc3
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04816475

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