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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diethyl Ether → HCID 178504336, 화합물

HRID 612431
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HRID 612431 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.CCOCC.C([Li])CCC.[Cl:24][Si:25](Cl)([CH3:27])[CH3:26]>CCCCCC>[Cl-:24].[CH3:26][SiH:25]([CH3:27])[CH:12]1[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5]2[C:13]1=[CH:1][CH:2]=[CH:3][CH:4]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl Ether2회HCID 6398DichlorodimethylsilaneHCID 6853FluoreneHCID 178418339Butyllithium

생성물 1

HCID 178504336HCID 178504336, 화합물수율 43%

시약·촉매·용매 1

HCID 8058Hexane용매

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온도
-10 °C

실험 절차

A 1 liter four-neck flask equipped with a reflux tube, a thermometer and a dropping funnel was thoroughly purged with nitrogen and dried. To the flask, fluorene (5.00 g, 30 mmol) and dehydrated ether (100 ml) were introduced. Under stirring at -10° C., a hexane solution of n-butyllithium (30 mmol) was dropwise added over a period of 30 minutes. After the dropwise addition, the temperature of the system was allowed to spontaneously and slowly rise to room temperature, followed by stirring at room temperature for 4 hours. The reaction liquid became a yellow slurry. The slurry was dropwise added to a dichlorodimethylsilane (18.24 ml, 150 mmol)/dehydrated ether (100 ml) solution under stirring at -10° C. over a period of 1 hour. After the temperature of the system was allowed to spontaneously rise to room temperature, the reaction mixture was stirred over night. Lithium chloride was removed by means of pressure filteration of the resulting solution using a glass filter (G-5). Further the solvent and the unreacted dichlorodimethylsilane remained in the filtrate were removed under reduced pressure. The resulting filtrate was reslurried with dehydrated hexane (100 ml) and subjected to pressure filteration using a glass filter (G-5) to obtain a white powder (3.30 g, yield: 43%).

후처리

  1. customA 1 liter four-neck flask equipped with a reflux tube
  2. customa thermometer and a dropping funnel was thoroughly purged with nitrogen
  3. customdried
  4. additionAfter the dropwise addition
  5. customslowly rise to room temperature
  6. stirringby stirring at room temperature for 4 hours
  7. customThe reaction liquid
  8. stirringunder stirring at -10° C. over a period of 1 hour
  9. customwas allowed to spontaneously rise to room temperature
  10. stirringthe reaction mixture was stirred over night
  11. customLithium chloride was removed by means of pressure filteration of the resulting solution
  12. filtrationfilter (G-5)
  13. customwere removed under reduced pressure
  14. filtrationfilter (G-5)

출처 및 근거

ORD 기록
ord-bf05d69a53894d82a7df6bfbec2ce79b
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06004897

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