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

HRID 541106

반응식

HRID 541106 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dc8c5e0dd9064b429536880dde457406
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871970B2

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