Titanocene dichioride → Dimethyl titanocene

HRID 567691

반응식

HRID 567691 반응식
[Cl-].[Cl-].[CH-:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH-:8]1[CH:12]=[CH:11][CH:10]=[CH:9]1.[Ti+2:13].C[Li]>CCOCC.O>[CH3:8][C-:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[C-:8]1([CH3:3])[CH:12]=[CH:11][CH:10]=[CH:9]1.[Ti+2:13]

참가 물질

5

반응물 2

HCID 124040768Titanocene dichiorideHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 129651941Dimethyl titanocene수율 197%

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매3회

실험 절차

A solution of 2.49 g (10.0 mmol) of titanocene dichloride in 50 ml of ether in the dark at 0° C. was treated with 17.5 ml of 1.4M methyllithium solution in ether maintaining the internal temperature below 5° C. The resulting yellow/orange mixture was stirred at room temperature for 30 minutes and the reaction was quenched by slowly adding 25 g of ice. The quenched reaction mixture was diluted with 50 ml of ether and 25 ml of water and the layers were separated. The organic layer was dried over magnesium sulfate and concentrated in vacuo to afford 2.03 g (98%) of the title compound as a light-sensitive solid. The dimethyl titanocene could be stored as a solution in toluene at 0° C. for at least 2 weeks without apparent chemical degradation. 1H NMR (200 MHz, CDCl3) δ−0.15 (6H, s), 6.06 (10H, s).

후처리

  1. customthe reaction was quenched
  2. additionby slowly adding 25 g of ice
  3. customThe quenched reaction mixture
  4. customthe layers were separated
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b375ef341df3436b8923fa8bc1a8587f
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06180624B2

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