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Tetraethoxysilane → Cyclopentyltriethoxysilane

HRID 1424697
ノート
印刷プレビュー

反応式

HRID 1424697 の反応式
C(O[Si:4]([O:11][CH2:12][CH3:13])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])C.[CH:14]1([Mg]Br)[CH2:18][CH2:17][CH2:16][CH2:15]1.[Cl-].[NH4+]>COC(C)(C)C>[CH:14]1([Si:4]([O:5][CH2:6][CH3:7])([O:8][CH2:9][CH3:10])[O:11][CH2:12][CH3:13])[CH2:18][CH2:17][CH2:16][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6517TetraethoxysilaneHCID 25517Ammonium ChlorideHCID 178419650HCID 178419650、化合物

生成物 1

HCID 16217491Cyclopentyltriethoxysilane

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

60 ml of dry t-butyl methyl ether and 14.0 gram (0.067 mole) of tetraethoxysilane were charged in a 250 ml flask equipped with a reflux condenser and a stirring apparatus in an atmosphere of nitrogen and the solution of cyclopentyl magnesium bromide prepared above under (a) was slowly added while keeping the internal temperature below 10° C. After completion of addition stirring was carried out at room temperature for 6 hours and at reflux temperature for 2 hours. To the resulting reaction mass 10-20 ml of saturated aqueous ammonium chloride solution was added drop wise to dissolve magnesium salt. The organic layer was separated from the aqueous layer, dried and evaporated to give crude cyclopentyltriethoxysilane. The crude was purified by fractional distillation under reduced pressure, yielding 12 gram of pure cyclopentyltriethoxysilane (76% of the theoretical maximum yield based on the amount of tetraethoxysilane).

後処理

  1. customequipped with a reflux condenser
  2. additionwas slowly added
  3. customthe internal temperature below 10° C
  4. additionAfter completion of addition
  5. temperatureat reflux temperature for 2 hours
  6. additionwas added drop wise
  7. customThe organic layer was separated from the aqueous layer
  8. customdried
  9. customevaporated
  10. customto give crude cyclopentyltriethoxysilane
  11. distillationThe crude was purified by fractional distillation under reduced pressure

出典と根拠

ORDレコード
ord-28d1341b6ee944a5a8a43f387b831c2a
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927753B2

反応ノート

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