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

HRID 129319노트

반응식

HRID 129319 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-37fdbc60cac44c15b76a3d911c671799
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466710

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