Sodium Hydroxide → 1-[2-(dimethylamino)ethoxy]-N,N,2-trimethylpropane-2-amine

HRID 541106

反応式

HRID 541106 の反応式
[OH-].[Na+].[CH3:3][N:4]([CH3:10])[C:5]([CH3:9])([CH3:8])[CH2:6][OH:7].Cl.[CH3:12][N:13]([CH3:17])[CH2:14][CH2:15]Cl>C1(C)C=CC=CC=1>[CH3:12][N:13]([CH3:17])[CH2:14][CH2:15][O:7][CH2:6][C:5]([CH3:9])([N:4]([CH3:10])[CH3:3])[CH3:8]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 234352-(Dimethylamino)-2-methylpropanolHCID 11636816N,N-Dimethylaminoethyl chloride hydrochloride

生成物 1

HCID 866576141-[2-(dimethylamino)ethoxy]-N,N,2-trimethylpropane-2-amine収率 27%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

To toluene (100 ml), sodium hydroxide (16.7 g, 418 mmol) and 2-dimethylamino-2-methyl-1-propanol (23.4 g, 200 mmol) were added and the mixture was heated at reflux for 2 hours. After cooling to 70° C., β-dimethylaminoethyl chloride hydrochloride (28.8 g, 200 mmol) was added. Then, the mixture was heated at reflux for 5.5 hours. After cooling to room temperature, insolubles were separated by filtration and the organic phase was concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 10.3 g (in a yield of 27%) of the objective compound as a colorless liquid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. temperatureThen, the mixture was heated
  4. temperatureat reflux for 5.5 hours
  5. temperatureAfter cooling to room temperature
  6. custominsolubles were separated by filtration
  7. concentrationthe organic phase was concentrated under reduced pressure
  8. distillationThe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-dc8c5e0dd9064b429536880dde457406
出典データセット
uspto-grants-2014_10
特許番号
US08871970B2

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