Diethylamine → (2,2-Diethoxyethyl)diethylamine

反応式

[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]

参加物

反応物 2

HCID 8021Diethylamine

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

生成物 1

HCID 77164(2,2-Diethoxyethyl)diethylamine収率 72.8%

反応条件

温度: 40 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード: ord-b8362daa2ff14d6793a2fdc37ea197da
出典データセット: uspto-grants-1985_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04533677

反応ノート

読み込み中…

参加物