1-Morpholinoethanol → HCID 13335983、化合物

HRID 979984ノート

反応式

HRID 979984 の反応式
[Cl:1][C:2]1[CH:11]=[C:6]([C:7]([O:9][CH3:10])=[O:8])[C:5]([OH:12])=[C:4]([C:13](=[O:16])[CH2:14][CH3:15])[CH:3]=1.[Na].[O:18]1[CH2:23][CH2:22][N:21]([CH:24](O)C)[CH2:20][CH2:19]1>>[Cl:1][C:2]1[CH:11]=[C:6]([C:7]([O:9][CH2:10][CH2:24][N:21]2[CH2:22][CH2:23][O:18][CH2:19][CH2:20]2)=[O:8])[C:5]([OH:12])=[C:4]([C:13](=[O:16])[CH2:14][CH3:15])[CH:3]=1

参加物

4

反応物 3

HCID 30293761-MorpholinoethanolHCID 5360545SodiumHCID 13335980HCID 13335980、化合物

生成物 1

HCID 13335983HCID 13335983、化合物収率 88.8%

実験手順

A 24.3 g (0.10 mole) quantity of methyl 5-chloro-3-propionylsalicylate was added to a solution of 0.5 g (0.022 mole) of sodium in 300 ml of morpholinoethanol. The mixture was maintained at room temperature for 24 hours and was heated at 2 hours at 90° C. The reaction mixture was subjected to distillation at reduced pressure to remove the excess unreacted morpholinoethanol and the methanol produced, and the residue was recrystallized from cyclohexane to obtain 38.0 g (88.8%) of crystals which melt at 144.0° to 146.3° C.

後処理

  1. temperaturewas heated at 2 hours at 90° C
  2. distillationThe reaction mixture was subjected to distillation at reduced pressure
  3. customto remove the excess unreacted morpholinoethanol
  4. customthe methanol produced
  5. customthe residue was recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-f478ea3b97504371bf9d97b2daa64432
出典データセット
uspto-grants-1987_01
特許番号
US04634768

反応ノート

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