Diethylaluminum chloride → HCID 16689304, 화합물

HRID 1293491

반응식

HRID 1293491 반응식
[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]

참가 물질

7

반응물 4

HCID 7277Diethylaluminum chlorideHCID 214031-EthoxynaphthaleneHCID 178418306HCID 178418306, 화합물HCID 178506782HCID 178506782, 화합물

생성물 1

HCID 16689304HCID 16689304, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8058Hexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f1f64abcf1c44fc987c528aa90604857
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238757B2

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