Imidazole → Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl-

HRID 1007468

반응식

HRID 1007468 반응식
CN(C)C=O.N1C=CN=C1.[CH3:11][C:12]([Si:15]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)Cl)([CH3:14])[CH3:13].[Br:29][C:30]1[CH:35]=[CH:34][C:33]([OH:36])=[CH:32][CH:31]=1>C1CCCCC1.CCOC(C)=O.CCCCC.C(OCC)(=O)C.O>[Br:29][C:30]1[CH:35]=[CH:34][C:33]([O:36][Si:15]([C:12]([CH3:14])([CH3:13])[CH3:11])([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:32][CH:31]=1

참가 물질

9

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 78084-BromophenolHCID 94078tert-Butyldiphenylchlorosilane

생성물 1

HCID 11292808Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl-

시약·촉매·용매 4

HCID 962Water용매HCID 8003Pentane용매HCID 8857Ethyl Acetate용매HCID 21867204Cyclohexane ethylacetate용매

실험 절차

400 ml of dimethylformamide, 31.18 g of imidazole and 125.89 g of 1,1-dimethyl-ethyldiphenyl-chlorosilane are added under an inert atmosphere and at ambient temperature to 80.89 g of parabromophenol, then the solution obtained is agitated for 2 hours. The reaction medium is poured into 2 litres of water, precipitation is observed, the solid is solubilized with ethyl acetate and the aqueous phase is extracted with ethyl acetate, the combined organic phases are dried and evaporated under reduced pressure until an oil is obtained. Pentane is added and crystallisation is observed. After filtration and drying of the precipitate 179.24 g of expected product is obtained. Rf: 0.53 (thin layer chromatography, support: silica, eluant Cyclohexane/AcOEt 95/5).

후처리

  1. customthe solution obtained
  2. extractionthe aqueous phase is extracted with ethyl acetate
  3. customthe combined organic phases are dried
  4. customevaporated under reduced pressure until an oil
  5. customis obtained
  6. customcrystallisation
  7. filtrationAfter filtration
  8. dry with materialdrying of the precipitate 179.24 g of expected product
  9. customis obtained

출처 및 근거

ORD 기록
ord-ccdf75384858493c97ca06472b9ed1a5
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06794415B2

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