Methylgallium dichloride → Bis-(3-dimethylaminopropyl)methylgallium

HRID 1458510ノート

反応式

HRID 1458510 の反応式
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][Li].[Cl-].[Cl-].[CH3:10][Ga+2:11]>CCCCC.C1C=CC=CC=1>[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][Ga:11]([CH2:5][CH2:4][CH2:3][N:2]([CH3:7])[CH3:1])[CH3:10]

参加物

5

反応物 2

HCID 178477772Methylgallium dichlorideHCID 178506872HCID 178506872、化合物

生成物 1

HCID 14531890Bis-(3-dimethylaminopropyl)methylgallium

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 8003Pentane溶媒

実験手順

5 g of 3-dimethylaminopropyllithium (53.7 mmol) are suspended in 40 ml of pentane, and a solution of 4 g of methylgallium dichloride (25.7 mmol) in 20 ml of benzene is added dropwise. The mixture is first stirred at room temperature for one hour and then boiled under reflux for 6 hours. After cooling, the lithium chloride and excess lithium salt are filtered off and the solvent is stripped off in vacuo. The residue which remains is sublimed in vacuo at an oil bath temperature of 60° C. Bis-(3-dimethylaminopropyl)methylgallium is obtained as a white solid of melting point 52° C.

後処理

  1. temperatureunder reflux for 6 hours
  2. temperatureAfter cooling
  3. filtrationthe lithium chloride and excess lithium salt are filtered off
  4. customThe residue which remains is sublimed in vacuo at an oil bath
  5. customtemperature of 60° C

出典と根拠

ORDレコード
ord-650a2a53f26c4523806b27c73bbb10e0
出典データセット
uspto-grants-1998_12
特許番号
US05851946

反応ノート

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