Hydrochloric Acid → 3-Fluoro-2-methylthionaphthacene-5,12-dione

HRID 359624

반응식

HRID 359624 반응식
[F:1][C:2]1[C:19](F)=[CH:18][C:17]2[C:16](=[O:21])[C:15]3[C:6](=[CH:7][C:8]4[C:13]([CH:14]=3)=[CH:12][CH:11]=[CH:10][CH:9]=4)[C:5](=[O:22])[C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:29][S-:30].[Na+].Cl>O1CCCC1>[F:1][C:2]1[C:19]([S:30][CH3:29])=[CH:18][C:17]2[C:16](=[O:21])[C:15]3[C:6]([C:5](=[O:22])[C:4]=2[CH:3]=1)=[CH:7][C:8]1[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH:14]=3

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 4378561Sodium methanethiolateHCID 200898342,3-Difluoronaphthacene-5,12-dione

생성물 1

HCID 200654153-Fluoro-2-methylthionaphthacene-5,12-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1 g (3.4 mmol) of 2,3-difluoronaphthacene-5,12-dione, 0.94 g (6.8 mmol) of potassium carbonate, 0.47 g (6.8 mmol) of sodium methanethiolate and 20 ml of tetrahydrofuran are stirred at 25° C. for 2.5 hours. The mixture is poured into dilute hydrochloric acid and extracted with THF/toluene. The organic phase is dried over sodium sulfate and evaporated. The residue is chromatographed on silica gel with toluene. Yield 0.55 g (50%); melting point 230°-235° C.

후처리

  1. extractionextracted with THF/toluene
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customevaporated
  4. customThe residue is chromatographed on silica gel with toluene

출처 및 근거

ORD 기록
ord-93a7efa5fd9e40e4a3b25ddb4ec45ece
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05001243

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