Sulfuric Acid → 5-(2-Benzylaminopropoxy)salicylamide

HRID 4554

反応式

HRID 4554 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 conc. sulfuric acid are added to a solution of 104.5 g of 5-(2-oxo-propoxy)salicylamide in 1000 ml of methanol, and the mixture is hydrogenated, in the presence of 3.0 g of a Pt/C catalyst under normal conditions until 1 equivalent of hydrogen has been absorbed. The catalyst is filtered off, and the solution is then stirred up with about 10 g of pulverised calcium carbonate; the mixture is again filtered, and concentrated by evaporation. The oil remaining behind crystallises from isopropanol. Repeated recrystallisation from isopropanol yields 5-[2-(benzylamino)-propoxy]-salicylamide, m.p. 102°-104°.

後処理

  1. customhas been absorbed
  2. filtrationThe catalyst is filtered off
  3. filtrationthe mixture is again filtered
  4. concentrationconcentrated by evaporation
  5. custombehind crystallises from isopropanol
  6. customrecrystallisation from isopropanol

出典と根拠

ORDレコード
ord-fd0ebe5400be4198acdf81230619e204
出典データセット
uspto-grants-1988_02
特許番号
US04727067

関連ノート

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