Gallium monochloride → Tris(2,2-dimethylpropyl)gallane

HRID 986091

반응식

HRID 986091 반응식
[Cl-].[Cl-].[Cl-].[Ga+3:4].[CH2:5]([Mg]Cl)[C:6]([CH3:9])([CH3:8])[CH3:7]>C(OCC)C>[CH2:5]([Ga: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]

참가 물질

4

반응물 2

HCID 186022Gallium monochlorideHCID 178418809HCID 178418809, 화합물

생성물 1

HCID 13742233Tris(2,2-dimethylpropyl)gallane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A flask charged with 9.578 g. (54.41 mmol) of freshly sublimed gallium trichloride dissolved in 250 ml. of dry diethyl ether (from sodium/benzophenone), was fitted with a condenser, mechanical stirrer and a pressure equalizing addition funnel. Under a cover of argon, 100 ml., 2.27M 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 gallium trichloride solution over a period of 20 min. After the addition was complete, the reaction mixture was stirred at room temperature for 18 hours. The stirrer, condenser and addition funnel were replaced by stoppers and S Teflon valve adapter. The diethyl ether was then removed by vacuum distillation at room temperature. The crude product, a trisneopentylgallium etherate mixture, was isolated by vacuum distillation at 125° C. into a sidearm flask (cooled to -196° C.) attached to the reaction flask by means of an 85° elbow. This distillation must be continued for approximately 5 hours. The diethyl ether was then removed from stirred, crude trisneopentyl gallium by simple vacuum distillation at room temperature for 1 hour. The product was finally purified by vacuum distillation in a short path still at 59.5° C. (0.01 mm, static vacuum). The yield of purified trisneopentyl gallium was 14.04 g (49.58 mmol, 91.1% based on gallium trichloride).

후처리

  1. additionA flask charged with 9.578 g
  2. additionaddition funnel
  3. customfrom purified neopentyl chloride and magnesium turnings)
  4. additionThe Grignard reagent was then added to the gallium trichloride solution over a period of 20 min
  5. additionAfter the addition
  6. additionThe stirrer, condenser and addition funnel
  7. customThe diethyl ether was then removed by vacuum distillation at room temperature

출처 및 근거

ORD 기록
ord-6984ad049e054dfa89fd93c25a090258
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04710575

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