Sodium Iodide → Silane, (5-iodo-1-pentynyl)trimethyl-

HRID 129319ノート

反応式

HRID 129319 の反応式
Cl[CH2:2][CH2:3][CH2:4][C:5]#[C:6][Si:7]([CH3:10])([CH3:9])[CH3:8].[I-:11].[Na+]>CC(=O)CC>[I:11][CH2:2][CH2:3][CH2:4][C:5]#[C:6][Si:7]([CH3:10])([CH3:9])[CH3:8]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 27579421-Chloro-5-(trimethylsilyl)-4-pentyne

生成物 1

HCID 11140046Silane, (5-iodo-1-pentynyl)trimethyl-収率 93.8%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 5-chloro-1-trimethylsilylpent-1-yne (13.5 g) and sodium iodide (29 g) in butanone (100 ml) was heated at reflux for 10 hours. After this time the solvent was removed in vacuo and the residue partitioned between diethyl ether and water. The organic phase was separated, washed with water and brine before drying over anhydrous magnesium sulphate. The solvent was removed under reduced pressure to leave 5-iodo-1-trimethylsilylpent-1-yne as a colourless oil (19.3 g).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 10 hours
  3. customAfter this time the solvent was removed in vacuo
  4. customthe residue partitioned between diethyl ether and water
  5. customThe organic phase was separated
  6. washwashed with water and brine
  7. dry with materialbefore drying over anhydrous magnesium sulphate
  8. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-37fdbc60cac44c15b76a3d911c671799
出典データセット
uspto-grants-1995_11
特許番号
US05466710

反応ノート

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