Hydrochloric Acid → 2-Fluoro-3-methoxy-naphthacene-5,12-dione

HRID 1196138

反応式

HRID 1196138 の反応式
F[C:2]1[C:19]([F:20])=[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:23](=O)([O-])[O-:24].[K+].[K+].CO.Cl>O1CCCC1>[F:20][C:19]1[C:2]([O:24][CH3:23])=[CH:3][C:4]2[C:5](=[O:22])[C:6]3[C:15](=[CH:14][C:13]4[C:8]([CH:7]=3)=[CH:9][CH:10]=[CH:11][CH:12]=4)[C:16](=[O:21])[C:17]=2[CH:18]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 11430Potassium CarbonateHCID 200898342,3-Difluoronaphthacene-5,12-dione

生成物 1

HCID 200898242-Fluoro-3-methoxy-naphthacene-5,12-dione収率 25%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1 g (3.4 mmol) of 2,3-difluoronaphthacene-5,12-dione, 0.94 g (6.8 mmol) of potassium carbonate, 3.24 g of methanol and 20 ml of tetrahydrofuran (THF) are stirred at 25° C. for 18 hours and under reflux for 3 days. The mixture is cooled and dilute hydrochloric acid is added. The product is filtered off, washed with water, dried and chromatographed with methylene chloride on silica gel. Sublimation under 1.3×10-1 bar/180°-310° C. gives 0.26 g (25%) of pure product, melting point >250° C.

後処理

  1. temperatureunder reflux for 3 days
  2. temperatureThe mixture is cooled
  3. filtrationThe product is filtered off
  4. washwashed with water
  5. customdried
  6. customchromatographed with methylene chloride on silica gel

出典と根拠

ORDレコード
ord-1c53d21c73d64d6cb8f7397ff5d7eb30
出典データセット
uspto-grants-1992_05
特許番号
US05112977

関連ノート

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