Dimethylamine → 1,2-Ethanediamine,N2-(1,1-dimethylethyl)-N1,N1-dimethyl-

HRID 1446024ノート

反応式

HRID 1446024 の反応式
Cl.[C:2]([NH:6][CH2:7][CH2:8]Cl)([CH3:5])([CH3:4])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[CH3:16][NH:17][CH3:18]>>[C:2]([NH:6][CH2:7][CH2:8][N:17]([CH3:18])[CH3:16])([CH3:5])([CH3:4])[CH3:3]

参加物

4

反応物 3

HCID 674DimethylamineHCID 11430Potassium CarbonateHCID 25021339HCID 25021339、化合物

生成物 1

HCID 206267161,2-Ethanediamine,N2-(1,1-dimethylethyl)-N1,N1-dimethyl-収率 56%

反応条件

温度
140 °C

実験手順

2-(t-Butylamino)ethylchloride hydrochloride (1.2 g, 7.0 mmol) is dissolved in aqueous dimethylamine solution (40% by weight, 22 mL) in a sealed tube. The mixture is heated in a 140° C. oil bath for six hours, allowed to cool to room temperature, and then is saturated with solid potassium carbonate. The mixture is extracted thrice with ethyl acetate. The combined extracts are dried over anhydrous sodium sulfate, decanted, and concentrated under reduced pressure to give N-t-butyl,N′,N′-dimethylethylenediamine as a light brown liquid (0.57 g, 56%). The crude material is carried on to the following step without further purification.

後処理

  1. temperatureto cool to room temperature
  2. extractionThe mixture is extracted thrice with ethyl acetate
  3. dry with materialThe combined extracts are dried over anhydrous sodium sulfate
  4. customdecanted
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-40f60a6a7aa94965977c1c9486393b81
出典データセット
uspto-grants-2010_02
特許番号
US07666901B2

反応ノート

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