Dimethylamine → 4-[2-(Dimethylamino)ethoxy]aniline

HRID 639373ノート

反応式

HRID 639373 の反応式
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][CH:6]=1.[CH3:12][NH:13][CH3:14]>[OH-].[Na+]>[CH3:12][N:13]([CH3:14])[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 1196994-(2-Chloroethoxy)aniline

生成物 1

HCID 64846554-[2-(Dimethylamino)ethoxy]aniline

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

11.15 g (0.065 Mol) of 4-(2-Chloro-ethoxy)-phenylamine is suspended in 150 mL (1.18 Mol) of dimethylamine (40% in water; Fluka 38940) and heated under stirring in a steel pressure reactor at 4 bar for 21 h. After cooling the reaction mixture is diluted with 150 mL of 2N NaOH and extracted with ethyl acetate. The combined organic layers are washed with water, dried (Na2SO4), filtered and evaporated under reduced pressure to obtain 4-(2-dimethylamino-ethoxy)-phenylamine. Title compound: ES-MS: 181 [M+H]+; single peak at tR=1.10 min (System 1).

後処理

  1. temperatureheated
  2. temperatureAfter cooling the reaction mixture
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layers are washed with water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-46ac115a262b4efd8020de82c5e98e43
出典データセット
uspto-grants-2010_04
特許番号
US07691855B2

反応ノート

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