Dimethyl Sulfate → Flosequinan

HRID 1155520ノート

反応式

HRID 1155520 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 4474062Flosequinan

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-47a90ed0e75b4d17b3f3b5b5c34ac574
出典データセット
uspto-grants-1981_11
特許番号
US04302460

反応ノート

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