Diethyl aluminum chloride → [2-(Dimethylamino)benzyl]-diethylaluminium

HRID 898104ノート

反応式

HRID 898104 の反応式
[Cl-].[CH2:2]([Al+:4][CH2:5][CH3:6])[CH3:3].[CH3:7][N:8]([CH3:17])[C:9]1[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=1[CH2:11][Li]>C1(C)C=CC=CC=1>[CH3:7][N:8]([CH3:17])[C:9]1[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=1[CH2:11][Al:4]([CH2:5][CH3:6])[CH2:2][CH3:3]

参加物

4

反応物 2

HCID 16686102Diethyl aluminum chlorideHCID 178506851HCID 178506851、化合物

生成物 1

HCID 18622320[2-(Dimethylamino)benzyl]-diethylaluminium収率 62%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

7.17 g (7.5 ml; 59.5 mmol) of diethylaluminium chloride were added dropwise to a suspension, cooled to −30° C., of 8.40 g (59.5 mmol) of 2-dimethylaminobenzyllithium in 150 ml of toluene in an inert nitrogen atmosphere. After slow warming to room temperature, the mixture was stirred for 15 hours in order to complete the reaction. Filtration through a D4 frit and removal of the solvent by distillation gave 8:05 g of [2-(dimethylamino)benzyl]-diethylaluminium (36.7 mmol/62%) as a colourless liquid by slow fractional distillation from the residue.

後処理

  1. customthe reaction
  2. filtrationFiltration
  3. customthrough a D4 frit and removal of the solvent
  4. distillationby distillation

出典と根拠

ORDレコード
ord-14dd28a1d06a4e529c6798f2863cf3f4
出典データセット
uspto-grants-2008_04
特許番号
US07351678B2

反応ノート

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