13510-35-5 → Indium, tris(2,2-dimethylpropyl)-

HRID 986092Notes

Reaction equation

HRID 986092 reaction equation
[I-].[I-].[I-].[In+3:4].[CH2:5]([Mg]Cl)[C:6]([CH3:9])([CH3:8])[CH3:7]>C(OCC)C>[CH2:5]([In:4]([CH2:5][C:6]([CH3:9])([CH3:8])[CH3:7])[CH2:5][C:6]([CH3:9])([CH3:8])[CH3:7])[C:6]([CH3:9])([CH3:8])[CH3:7]

Participants

4

Reactant 2

HCID 1117945613510-35-5HCID 178418809HCID 178418809, compound

Product 1

HCID 11049023Indium, tris(2,2-dimethylpropyl)-

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A flask, charged with 29.13 g (58.3 mmol) of indium triiodide dissolved in 100 ml. of dry diethyl ether (from sodium/benzophenone) was fitted with a condenser, magnetic stir bar and a pressure equalizing addition funnel. Under a cover of argon, 100 ml., 2.32M neopentyl magnesium chloride in diethyl ether solution (previously prepared from purified neopentyl chloride and magnesium turnings) was transferred to the addition funnel. The Grignard reagent was then added to the indium triiodide solution over a period of 20 minutes. After the addition was complete, the reaction mixture was stirred at room temperature for 18 hours. The condenser and addition funnel were then replaced by a stopper and a S Teflon valve adapter and the diethyl ether was removed by vacuum distillation at room temperature. The crude product, a trisneopentyl indium etherate mixture, was isolated by vacuum distillation at 110° C. into a side-arm flask (cooled to -196° C.) attached to the reaction flask by means of an 85° elbow. The distillation must be continued for approximately 8 hours. The diethyl ether was then removed from the crude trisneopentyl indium by simple vacuum distillation at room temperature for 12 hours. The product, a crystalline solid was finally purified by vacuum sublimation at 30° C. with the receiving flask at -10° C. The yield of purified trisneopentyl indium was 17.7 g (53.9 mmol, 92.4% based on indium triiodide).

Workup

  1. dissolutiondissolved in 100 ml
  2. additionaddition funnel
  3. customfrom purified neopentyl chloride and magnesium turnings)
  4. additionThe Grignard reagent was then added to the indium triiodide solution over a period of 20 minutes
  5. additionAfter the addition
  6. additionThe condenser and addition funnel
  7. customa S Teflon valve adapter and the diethyl ether was removed by vacuum distillation at room temperature

Sources & evidence

ORD record
ord-1194a4dca0a345d3affb2afc3e91c12e
Source dataset
uspto-grants-1987_12
Patent number
US04710575

Reaction notes

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