INDIUM(III) IODIDE → Indium, tris(2,2-dimethylpropyl)-

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., 2.32 M neopentyl magnesium chloride in diethyl ether solutin (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 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, is 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).

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. customthe diethyl ether was removed by vacuum distillation at room temperature

ORDレコード

ord-8993471ee0b34d3d8f215095d0034754

出典データセット

uspto-grants-1986_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04621147