Pyridine → 6-((2-Ethylhexyl)(phenyl)amino)hexyl acetate

HRID 607491ノート

反応式

HRID 607491 の反応式
[CH2:1]([CH:3]([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:4][N:5]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][OH:12])[CH3:2].[C:23](OC(=O)C)(=[O:25])[CH3:24].N1C=CC=CC=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>ClCCl.O>[C:23]([O:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][N:5]([CH2:4][CH:3]([CH2:1][CH3:2])[CH2:19][CH2:20][CH2:21][CH3:22])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:25])[CH3:24]

参加物

7

反応物 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 24436Sodium SulfateHCID 670462816-((2-Ethylhexyl)(phenyl)amino)hexan-1-ol

生成物 1

HCID 578577296-((2-Ethylhexyl)(phenyl)amino)hexyl acetate収率 93.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

6-((2-ethylhexyl)(phenyl)amino)hexan-1-ol (8.0 g, 0.023 mol) and dichloromethane (100 ml) were loaded into a three-neck flask, stirred, and added with acetic anhydride (2.8 g, 0.028 mol) and pyridine (3.0 g, 0.038 mol). The mixture was allowed to react at 40° C. for 12 hours with stirring. The reaction product was transferred into a separate funnel, and was then added with water and dichloromethane, after which the organic layer was isolated therefrom, dehydrated using sodium sulfate, and then distilled under reduced pressure. Subsequently, the obtained viscous liquid was separated through silica column chromatography, thus obtaining 7.5 g of a yellowish transparent liquid.

後処理

  1. customto react at 40° C. for 12 hours
  2. stirringwith stirring
  3. customThe reaction product was transferred into a separate funnel
  4. customafter which the organic layer was isolated
  5. distillationdistilled under reduced pressure
  6. customSubsequently, the obtained viscous liquid was separated through silica column chromatography

出典と根拠

ORDレコード
ord-f3b9171a85224812a8fd2acec1063b2c
出典データセット
uspto-grants-2011_03
特許番号
US07915428B2

反応ノート

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