Triethylamine → N-(2,4-Dichlorophenyl)-3-(phenylmethoxy)benzeneacetamide

HRID 2114735ノート

反応式

HRID 2114735 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:10]1([CH2:16][O:17][C:18]2[CH:19]=[C:20]([CH2:24][C:25](Cl)=[O:26])[CH:21]=[CH:22][CH:23]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:3]=1[NH:4][C:25](=[O:26])[CH2:24][C:20]1[CH:21]=[CH:22][CH:23]=[C:18]([O:17][CH2:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:19]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 111232,4-DichloroanilineHCID 516892Sodium BicarbonateHCID 118178352-[3-(Phenylmethoxy)phenyl]acetyl Chloride

生成物 1

HCID 23440745N-(2,4-Dichlorophenyl)-3-(phenylmethoxy)benzeneacetamide収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2,4-dichloroaniline (2.67 g, 0.0165 mol) in dichloromethane (20 ml) was slowly added a solution of 2-[3-(phenylmethoxy)phenyl]acetyl chloride (3.84 g, 0.015 mol) in dichloromethane (10 ml). After stirring for three hours, triethylamine (2 ml, 0.015 mol) was added to the reaction and the reaction was allowed to stir overnight. To the reaction was added an aqueous solution of sodium bicarbonate. The mixture was extracted with dichloromethane. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated. The solid was triturated with ether and hexane, then filtered to provide the title compound (4.0 g, 70% yield): ES-MS (m/z) 372 [M+H]+.

後処理

  1. stirringto stir overnight
  2. extractionThe mixture was extracted with dichloromethane
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe solid was triturated with ether and hexane
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-e9302f6c18044f1e991ea721585fa783
出典データセット
uspto-grants-2008_10
特許番号
US07435729B2

反応ノート

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