Diethylaluminum chloride → HCID 16689304、化合物

HRID 1293491

反応式

HRID 1293491 の反応式
[Al:1](Cl)([CH2:4][CH3:5])[CH2:2][CH3:3].[CH2:7]([O:9][C:10]1([Li])[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12][CH2:11]1)[CH3:8].C([Li])(C)(C)C.C(OC1C2C(=CC=CC=2)C=CC=1)C>CCCCCC.C(OCC)C>[CH2:7]([O:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19]=1[C:18]([Al:1]([CH2:4][CH3:5])[CH2:2][CH3:3])=[CH:17][CH:16]=[CH:15]2)[CH3:8]

参加物

7

反応物 4

HCID 7277Diethylaluminum chlorideHCID 214031-EthoxynaphthaleneHCID 178418306HCID 178418306、化合物HCID 178506782HCID 178506782、化合物

生成物 1

HCID 16689304HCID 16689304、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

2.5 ml (20 mmol) of Et2AlCl are added dropwise at −40° C. to a suspension of 50 ml of diethyl ether and 3.5 g (20 mmol) of (1-ethoxynaphth-1-yl)lithium, prepared from 33 ml (56 mmol) of t-butyllithium (1.7M solution in pentane) and 9.7 g (56 mmol) of 1-ethoxynaphthalene in 200 ml of hexane. The mixture is slowly brought to room temperature and stirred at room temperature for 24 h. The mixture is subsequently decanted off from the solid, the solvent is removed, the residue is taken up in 35 ml of toluene and filtered through a D4 frit. After removal of the toluene, fractional distillation gives (8-ethoxynaphth-1-yl)diethylaluminium as pale-yellow liquid having a boiling point of 146° C. at 0.01 mbar.

後処理

  1. customis slowly brought to room temperature
  2. customThe mixture is subsequently decanted off from the solid
  3. customthe solvent is removed
  4. filtrationfiltered through a D4 frit
  5. customAfter removal of the toluene, fractional distillation

出典と根拠

ORDレコード
ord-f1f64abcf1c44fc987c528aa90604857
出典データセット
uspto-grants-2007_07
特許番号
US07238757B2

関連ノート

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