Diethyl Ether → AlH(CH2CH2CH2NMe2)2

反応式

[AlH3:1].[N:2]([CH3:6])([CH3:5])[CH2:3][CH3:4].[Li][CH2:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12].[CH2:14](OCC)C>>[AlH:1]([CH2:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12])[CH2:14][CH2:4][CH2:3][N:2]([CH3:6])[CH3:5]

参加物

反応物 4

HCID 3283Diethyl Ether

HCID 11723Dimethylethylamine

HCID 14488Aluminum hydride

HCID 178506872HCID 178506872、化合物

生成物 1

HCID 131725248AlH(CH2CH2CH2NMe2)2

反応条件

温度: -70 °C

実験手順

A dried flask is charged with AlH3.NEtMe2 (6.60 g, 64 mmol) under an inert atmosphere (e.g., argon) and then 50 mL of diethyl ether. The resulting slurry is cooled to −70° C. and a solution of LiCH2CH2CH2NMe2 (260 mL of 0.5 M solution in diethyl ether) is added. The resulting mixture is allowed to warm slowly to room temperature and stirred for 18 hours. The solvent is then removed in vacuo and the crude product is transferred to a smaller distillation apparatus for purification by distillation under vacuum.

後処理

temperatureto warm slowly to room temperature
customThe solvent is then removed in vacuo
distillationthe crude product is transferred to a smaller distillation apparatus for purification by distillation under vacuum

出典と根拠

ORDレコード: ord-b14a1194f1374959a711274ee62c8030
出典データセット: uspto-grants-2005_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06979370B2

反応ノート

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