2-(Methylamino)ethanol → 2-[N-[Bis-(4-chlorophenyl)methyl]N-methylamino]ethanol

HRID 1700888ノート

反応式

HRID 1700888 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](Cl)[C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[CH3:17][NH:18][CH2:19][CH2:20][OH:21].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[N:18]([CH2:19][CH2:20][OH:21])[CH3:17])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 80162-(Methylamino)ethanolHCID 11430Potassium CarbonateHCID 130784,4'-Dichlorobenzhydryl chloride

生成物 1

HCID 183189972-[N-[Bis-(4-chlorophenyl)methyl]N-methylamino]ethanol収率 79%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 4,4′-dichlorobenzhydryl chloride (5.20 g, 19.1 mmol) and 2-(methylamino)ethanol (9.0 g, 0.106 mol) in acetonitrile (100 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture was heated under reflux for 4 h. The cooled mixture was filtered and the filtrate was concentrated in vacuo. The residual oil was diluted with ethyl acetate, washed with water and brine and then dried over anhydrous magnesium sulfate. Evaporation of the solvent in vacuo followed by chromatography on silica gel (elution toluene-ethyl acetate 9:1) gave 4.29 g (79%) of the title material as a white solid: mp 49-50° C.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 4 h
  3. filtrationThe cooled mixture was filtered
  4. concentrationthe filtrate was concentrated in vacuo
  5. additionThe residual oil was diluted with ethyl acetate
  6. washwashed with water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customEvaporation of the solvent in vacuo

出典と根拠

ORDレコード
ord-bf06e1f2c1794fb4bfe16525fc26531c
出典データセット
uspto-grants-2002_02
特許番号
US06350892B1

反応ノート

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