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HCID 11244270、化合物 → HCID 9851847、化合物

HRID 1723475
ノート
印刷プレビュー

反応式

HRID 1723475 の反応式
[Br-].[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][N+:12]([CH3:15])=[CH:11][C:10]=2[C:16]([O:18][CH3:19])=[O:17])=[CH:5][CH:4]=1>C(O)C.[Pt]=O>[F:2][C:3]1[CH:8]=[CH:7][C:6]([C@H:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][C@H:10]2[C:16]([O:18][CH3:19])=[O:17])=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 11244270HCID 11244270、化合物

生成物 1

HCID 9851847HCID 9851847、化合物収率 98.8%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 702Ethanol溶媒

実験手順

4-(4'-Fluorophenyl)-3-methoxycarbonyl-1-methylpyridinium bromide (15.90 g), prepared as in Example 1, in ethanol (250 ml) was hydrogenated at atmospheric pressure and 45° for 24 hours, in the presence of platinum oxide (0.5 g). Evaporation of the filtrate after removing the catalyst gave a dark oil which was partitioned between 10% sodium carbonate solution (100 ml) and dichloromethane (30 ml). After separation, the aqueous phase was extracted with dichloromethane (3×20 ml) and the organic solutions dried (potassium carbonate) and evaporated to give an off-white solid (12.1 g). Crystallisation from ethyl acetate gave the title compound as white crystals (8.32 g, 72%), m.p. 88°-89°.

後処理

  1. customEvaporation of the filtrate
  2. customafter removing the catalyst
  3. customgave a dark oil which
  4. customwas partitioned between 10% sodium carbonate solution (100 ml) and dichloromethane (30 ml)
  5. customAfter separation
  6. extractionthe aqueous phase was extracted with dichloromethane (3×20 ml)
  7. dry with materialthe organic solutions dried (potassium carbonate)
  8. customevaporated

出典と根拠

ORDレコード
ord-6d9cb9680a45440a8f22afdfb477697d
出典データセット
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04861893

反応ノート

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