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Chloropentamethyldisilane → HCID 19812441, 화합물

HRID 373353
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HRID 373353 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

HCID 19812441HCID 19812441, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 13387N-methyl-2-pyrrolidone용매2회

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4440e051989445bca1c6b899bbdc701a
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05162559

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