Dichlorodimethylsilane → Silane, chloro(1-indenyl)dimethyl-

HRID 1953949Notes

Reaction equation

HRID 1953949 reaction equation
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.C([Li])CCC.[CH3:15][Si:16]([CH3:19])(Cl)[Cl:17]>CCCCCC>[CH3:15][Si:16]([Cl:17])([CH3:19])[CH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1

Participants

5

Procedure

In a 2-liter flask were charged 50 g (0.43 mol) of indene and 600 ml of dry n-hexane, to which was dripped down 270 ml of a hexane solution of 1.6 M n-butyllithium at 0° C. The mixture was stirred at room temperature for 10 hours, to which was added 111 g (0.86 mol) of dimethyidichlorosilane and the mixture was stirred as was at room temperature for 3 hours. After it was filtered through a G-4 filter, the reaction mixture was distilled under reduced pressure to remove volatile components. The crude product thus obtained was purified by distillation under reduced pressure (100° C., 7 mmHg) under argon atmosphere. As a result, 78 g of the target compound was obtained. Yield: 87%.

Workup

  1. stirringthe mixture was stirred
  2. waitas was at room temperature for 3 hours
  3. filtrationAfter it was filtered through a G-4
  4. filtrationfilter
  5. distillationthe reaction mixture was distilled under reduced pressure
  6. customto remove volatile components
  7. customThe crude product thus obtained
  8. distillationwas purified by distillation under reduced pressure (100° C., 7 mmHg) under argon atmosphere

Sources & evidence

ORD record
ord-0d9b415e2049402e8f6684984264b732
Source dataset
uspto-grants-2000_09
Patent number
US06121182

Reaction notes

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