Ethyl formate → 1,3-Bis(trimethylsilyl)propan-2-ol

HRID 610400ノート

反応式

HRID 610400 の反応式
C([O:3][CH2:4][CH3:5])=O.[CH3:6][Si:7]([CH2:10][Mg]Cl)([CH3:9])[CH3:8].Cl.[NH4+]>C(OCC)C>[CH3:6][Si:7]([CH3:10])([CH3:9])[CH2:8][CH:4]([OH:3])[CH2:5][Si:7]([CH3:9])([CH3:8])[CH3:6]

参加物

5

反応物 3

HCID 8025Ethyl formateHCID 21905121Ammonium hydrochlorideHCID 178418680HCID 178418680、化合物

生成物 1

HCID 126567131,3-Bis(trimethylsilyl)propan-2-ol収率 70%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Ethyl formate (0.1 mol) was slowly added to 0.3 mol of trimethylsilylmethyl magnesium chloride solution dissolved in diethyl ether which was contained in a 500 ml flask. The mixture was allowed to react under reflux for about 24 hours. After hydrolyzing the reactant using ammonium hydrochloride solution, the obtained reaction product was separated and purified by a vacuum distillation and a 70 percent yield was obtained. The structure of the obtained distillates was analyzed using NMR and a spectroscopic method of FT-IR spectroscopy.

後処理

  1. customwas contained in a 500 ml flask
  2. customto react
  3. temperatureunder reflux for about 24 hours
  4. customthe obtained reaction product
  5. customwas separated
  6. distillationpurified by a vacuum distillation
  7. customa 70 percent yield was obtained

出典と根拠

ORDレコード
ord-169259283d3540b3b4ec943f1d644776
出典データセット
uspto-grants-1999_12
特許番号
US05998557

反応ノート

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