Aluminium lithium hydride → Phosphine, bis(1,1-dimethylethyl)-

HRID 2410630ノート

反応式

HRID 2410630 の反応式
[Cl-].[C:2]([PH:6][C:7]([CH3:10])([CH3:9])[CH3:8])([CH3:5])([CH3:4])[CH3:3].[H-].[H-].[H-].[H-].[Li+].[Al+3]>CCOCC>[C:2]([PH:6][C:7]([CH3:10])([CH3:9])[CH3:8])([CH3:5])([CH3:4])[CH3:3]

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 22613607Di-tert-butylphosphine chloride

生成物 1

HCID 136643Phosphine, bis(1,1-dimethylethyl)-

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Di-tert-butylphosphine chloride (34 g, 188.41 mmol) was added to a Schlenk flask followed by diethyl ether (200 ml). The ether solution was cooled in a cold water bath and LiAlH4 (1M in diethyl ether, 100 ml, 100 mmol) was added slowly. This gave a yellow suspension which was allowed to stir at room temperature overnight. The suspension was quenched by the water (50 ml, degassed with nitrogen for 20 minutes). This gave a biphasic solution. The upper (organic layer) was cannula transferred into a clean Schlenk and the aqueous residues washed with a further 100 ml of ether. The ether extracts were combined and dried with sodium sulphate. The ether extracts were then cannula transferred into a clean Schlenk and the ether removed by distillation. This gave a colourless oil. Yield=22.0 g, 80%. 31P {1H} NMR (161.9 MHz, CDCl3): δ 21.0 ppm

後処理

  1. customThis gave a yellow suspension which
  2. customThe suspension was quenched by the water (50 ml, degassed with nitrogen for 20 minutes)
  3. customThis gave a biphasic solution
  4. customtransferred into a clean Schlenk
  5. washthe aqueous residues washed with a further 100 ml of ether
  6. dry with materialdried with sodium sulphate
  7. customcannula transferred into a clean Schlenk
  8. customthe ether removed by distillation
  9. customThis gave a colourless oil

出典と根拠

ORDレコード
ord-d26f4ea7b28d46d69e4ca136c7421de1
出典データセット
uspto-grants-2014_08
特許番号
US08816113B2

反応ノート

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