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 5 N 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 5 N 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-88f029f0c1fc4de69ced9fe1a375e41f
출처 데이터셋: uspto-grants-1988_11
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04788335

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