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Chloropentamethyldisilane → HCID 19812441、化合物

HRID 373353
ノート
印刷プレビュー

反応式

HRID 373353 の反応式
Br[CH:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4].[CH3:8][Si:9]([CH3:15])([CH3:14])[Si:10]([CH3:13])([CH3:12])Cl>[Zn].CN1CCCC1=O>[CH3:12][Si:10]([CH3:13])([CH:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4])[Si:9]([CH3:15])([CH3:14])[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 73795ChloropentamethyldisilaneHCID 954632(3H)-Furanone, 3-bromodihydro-

生成物 1

HCID 19812441HCID 19812441、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 13387N-methyl-2-pyrrolidone溶媒2 回

反応条件

温度
60 °C

実験手順

200 ml of N-methylpyrrolidone and 34.3 g of zinc dust are placed in a 1,000 ml three-neck flask fitted with internal thermometer, cold-drawn precision glass stirrer and dropping funnel. A mixture of 82.5 g of 2-bromo-γ-butyrolactone and 83.4 g of pentamethylchlorodisilane and 100 ml of N-methylpyrrolidone is added dropwise while stirring so that the internal temperature adjusts to 60° C. during the exothermic reaction. Stirring is continued for a further 6 h at this temperature and the reaction mixture is then poured onto 500 g of flaked ice. Once the ice has melted, the organic phase which separates is separated off and the aqueous phase is extracted with 200 ml of cyclohexane. The combined organic phases are distilled off using a rotary evaporator after drying over magnesium sulfate and the residue is distilled in vacuo.

後処理

  1. customfitted with internal thermometer, cold-drawn precision glass stirrer
  2. additionis added dropwise
  3. stirringStirring
  4. customthe organic phase which separates is separated off
  5. extractionthe aqueous phase is extracted with 200 ml of cyclohexane
  6. distillationThe combined organic phases are distilled off
  7. customa rotary evaporator
  8. dry with materialafter drying over magnesium sulfate
  9. distillationthe residue is distilled in vacuo

出典と根拠

ORDレコード
ord-4440e051989445bca1c6b899bbdc701a
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05162559

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート