Sulfuric Acid → 5-(2-Benzylaminopropoxy)salicylamide

HRID 615212

反応式

HRID 615212 の反応式
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(=O)(=O)(O)O.O=[C:15]([CH3:28])[CH2:16][O:17][C:18]1[CH:26]=[C:22]([C:23]([NH2:25])=[O:24])[C:21]([OH:27])=[CH:20][CH:19]=1.[H][H]>CO.[Pt]>[CH2:1]([NH:8][CH:15]([CH3:28])[CH2:16][O:17][C:18]1[CH:26]=[C:22]([C:23]([NH2:25])=[O:24])[C:21]([OH:27])=[CH:20][CH:19]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 7504BenzylamineHCID 137543335-(2-Oxopropoxy)salicylamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 137543345-(2-Benzylaminopropoxy)salicylamide

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 887Methanol溶媒

実験手順

55 g of benzylamine and 1.25 g of concentrated sulphuric acid are added to a solution of 104.5 g of 5-(2-oxopropoxy)salicylamide in 1000 ml of methanol and hydrogenated in the presence of 3.0 g of Pt/C-catalyst at room temperature and atmospheric pressure until 1 equivalent of hydrogen has been absorbed. The catalyst is filtered off, approximately 10 g of powdered calcium carbonate are stirred into the solution and the solution is filtered again and concentrated by evaporation. The oil remaining crystallises from isopropanol. Repeated recrystallisation from isopropanol yields 5-[2-(benzylamino)propoxy]salicylamide having a melting point of 102°-104°.

後処理

  1. filtrationThe catalyst is filtered off
  2. filtrationthe solution is filtered again
  3. concentrationconcentrated by evaporation
  4. customThe oil remaining crystallises from isopropanol
  5. customrecrystallisation from isopropanol

出典と根拠

ORDレコード
ord-63de6bddd2414f74b745644984c3ffc9
出典データセット
uspto-grants-1985_02
特許番号
US04497813

関連ノート

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