Bis(isobutyl)aluminum chloride → (2-Methoxybenzyl)diisobutylaluminium

HRID 1293492ノート

反応式

HRID 1293492 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH2:5][Mg]Cl.[Al:12](Cl)([CH2:17][CH:18]([CH3:20])[CH3:19])[CH2:13][CH:14]([CH3:16])[CH3:15]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH2:5][Al:12]([CH2:17][CH:18]([CH3:20])[CH3:19])[CH2:13][CH:14]([CH3:16])[CH3:15]

参加物

4

反応物 2

HCID 15688Bis(isobutyl)aluminum chlorideHCID 178489472HCID 178489472、化合物

生成物 1

HCID 16688367(2-Methoxybenzyl)diisobutylaluminium

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

150 ml (39 mmol) of (2-methoxybenzyl)magnesium chloride as 0.26 molar solution are added dropwise over the course of 3 hours at 0° C. to 6.83 g (38.7 mmol) of iBu2AlCl in 250 ml of tetrahydrofuran. The mixture is slowly brought to room temperature and stirred at room temperature for 18 h. The solvent is removed under reduced pressure (0.05 mbar), and the residue is suspended in 125 ml of n-pentane. The mixture is subsequently filtered through a D4 frit. After removal of the n-pentane, fractional distillation gives (2-methoxybenzyl)diisobutylaluminium as colourless, viscous liquid having a boiling point of 85° C. at 0.05 mbar.

後処理

  1. customis slowly brought to room temperature
  2. customThe solvent is removed under reduced pressure (0.05 mbar)
  3. filtrationThe mixture is subsequently filtered through a D4 frit
  4. customAfter removal of the n-pentane, fractional distillation

出典と根拠

ORDレコード
ord-058f60cc42c7472195cce5a8c5c06ca4
出典データセット
uspto-grants-2007_07
特許番号
US07238757B2

反応ノート

読み込み中…