Diethylamine → (2,2-Diethoxyethyl)diethylamine

반응식

[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5]Br)[CH3:2].[CH2:10]([NH:12][CH2:13][CH3:14])[CH3:11]>>[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][N:12]([CH2:13][CH3:14])[CH2:10][CH3:11])[CH3:2]

참가 물질

반응물 2

HCID 8021Diethylamine

HCID 74852Ethane, 2-bromo-1,1-diethoxy-

생성물 1

HCID 77164(2,2-Diethoxyethyl)diethylamine수율 72.8%

반응 조건

온도: 40 °C

실험 절차

Bromoacetaldehyde diethylacetal, 52.4 g (0.26 mol), was mixed carefully with approximately 70.7 g (0.967 mol) diethylamine and stirred at 40° C. overnight. The reaction mixture was concentrated under reduced pressure and the residue dissolved in water and basified with cold 5N sodium hydroxide. The reaction mixture was extracted twice with diethyl ether, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a tan oil. Distillation gave 35.8 g (72.8%) diethylaminoacetaldehyde diethylacetal as a clear liquid. B.p. 65°-75° C. @ 1.0 mmHg.

후처리

concentrationThe reaction mixture was concentrated under reduced pressure
dissolutionthe residue dissolved in water and basified with cold 5N sodium hydroxide
extractionThe reaction mixture was extracted twice with diethyl ether
dry with materialdried over anhydrous sodium sulfate
concentrationconcentrated under reduced pressure
customto give a tan oil
distillationDistillation

출처 및 근거

ORD 기록: ord-b8362daa2ff14d6793a2fdc37ea197da
출처 데이터셋: uspto-grants-1985_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04533677

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