Titanocene dichioride → Dimethyl titanocene

HRID 399748

反応式

HRID 399748 の反応式
[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]

参加物

5

反応物 2

HCID 124040768Titanocene dichiorideHCID 178418348HCID 178418348、化合物

生成物 1

HCID 129651941Dimethyl titanocene収率 197%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒3 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d61f4d80d4f142d7925bc79b841615bf
出典データセット
uspto-grants-1998_10
特許番号
US05824678

関連ノート

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