Dimethyl Sulfate → Flosequinan

HRID 1155520노트

반응식

HRID 1155520 반응식
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:15])[CH:7]([S:12]([CH3:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1.[C:16](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(=O)CC>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:15])[C:7]([S:12]([CH3:14])=[O:13])=[CH:8][N:9]2[CH3:16])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 705794307-Fluoro-3-methylsulphinyl-4-quinolone

생성물 1

HCID 4474062Flosequinan

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

7-Fluoro-3-methylsulphinyl-4-quinolone (5.0 g.) was dissolved in hot butanone (250 ml.) containing anhydrous potassium carbonate (3.06 g.). The resulting suspension was stirred and treated dropwise with dimethyl sulphate (2.09 ml.). The mixture was stirred and boiled under reflux for 1 hour and filtered while hot. The filtrate was allowed to cool, giving a crystalline product. The product was collected and dried to give 7-fluoro-1-methyl-3-methylsulphinyl-4-quinolone, m.p. 226°-8°.

후처리

  1. stirringThe mixture was stirred
  2. temperatureunder reflux for 1 hour
  3. filtrationfiltered while hot
  4. temperatureto cool
  5. customgiving a crystalline product
  6. customThe product was collected
  7. customdried

출처 및 근거

ORD 기록
ord-47a90ed0e75b4d17b3f3b5b5c34ac574
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04302460

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