Sodium Carbonate → (2-Allyloxy-3-tert-butyl-5-methylphenyl)(2,7-di-tert-butylfluoren-9-yl)dimethylsilane

HRID 661763노트

반응식

HRID 661763 반응식
[H-].[K+].[C:3]([C:7]1[CH:19]=[CH:18][C:17]2[C:16]3[C:11](=[CH:12][C:13]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:14][CH:15]=3)[CH2:10][C:9]=2[CH:8]=1)([CH3:6])([CH3:5])[CH3:4].[CH2:24]([O:27][C:28]1[C:33]([C:34]([CH3:37])([CH3:36])[CH3:35])=[CH:32][C:31]([CH3:38])=[CH:30][C:29]=1[Si:39](Cl)([CH3:41])[CH3:40])[CH:25]=[CH2:26].C(=O)([O-])O.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>CCCCCC.O1CCCC1.C1(C)C=CC=CC=1>[CH2:24]([O:27][C:28]1[C:33]([C:34]([CH3:35])([CH3:36])[CH3:37])=[CH:32][C:31]([CH3:38])=[CH:30][C:29]=1[Si:39]([CH:10]1[C:9]2[CH:8]=[C:7]([C:3]([CH3:6])([CH3:5])[CH3:4])[CH:19]=[CH:18][C:17]=2[C:16]2[C:11]1=[CH:12][C:13]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:14][CH:15]=2)([CH3:40])[CH3:41])[CH:25]=[CH2:26]

참가 물질

9

반응물 5

HCID 10340Sodium CarbonateHCID 82127Potassium hydride2회HCID 516892Sodium BicarbonateHCID 40900822,7-Di-tert-butylfluoreneHCID 21880918(2-Allyloxy-3-tert-butyl-5-methylphenyl)chlorodimethylsilane

생성물 1

HCID 69233633(2-Allyloxy-3-tert-butyl-5-methylphenyl)(2,7-di-tert-butylfluoren-9-yl)dimethylsilane

시약·촉매·용매 3

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매3회HCID 8058Hexane용매

실험 절차

There was washed 3.00 g (22.45 mmol) of potassium hydride having a purity of 30% by weight with each 6 mL of hexane three times in an atmosphere of nitrogen, and 32 mL of tetrahydrofuran (referred to as “THF” hereinafter) was added thereto. To the obtained THF slurry of potassium hydride, 5.00 g (17.96 mml) of 2,7-di-tert-butylfluorene was added dropwise at 0° C. using 32 mL of a THF solution thereof. The obtained mixture was stirred for 2.5 hours at a room temperature, and then 5.33 g (17.96 mmol) of (2-allyloxy-3-tert-butyl-5-methylphenyl)chlorodimethylsilane was added dropwise at −78° C. using 6 mL of a toluene solution thereof. The temperature of the obtained liquid reaction mixture was raised up to a room temperature, and the mixture was stirred for 2.5 hours. The mixture was added dropwise at 0° C. to a mixture of 32 mL of a 10% aqueous solution of sodium hydrogen carbonate and 32 mL of a 10% aqueous solution of sodium carbonate, and the resultant mixture was extracted with 20 mL of toluene. The obtained extract was dried over sodium sulfate, and the solvent contained therein was distilled away under a reduced pressure, thereby obtaining quantitatively (2-allyloxy-3-tert-butyl-5-methylphenyl)(2,7-di-tert-butylfluoren-9-yl)dimethylsilane.

후처리

  1. additionwas added
  2. customThe temperature of the obtained liquid reaction mixture
  3. temperaturewas raised up to a room temperature
  4. stirringthe mixture was stirred for 2.5 hours
  5. extractionthe resultant mixture was extracted with 20 mL of toluene
  6. extractionThe obtained extract
  7. dry with materialwas dried over sodium sulfate
  8. distillationthe solvent contained therein was distilled away under a reduced pressure

출처 및 근거

ORD 기록
ord-e27859e77d314be686fb0976ff0ccdd8
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084559B2

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