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

HRID 412845

反応式

HRID 412845 の反応式
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

参加物

9

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 8003Pentane溶媒HCID 8857Ethyl Acetate溶媒HCID 21867204Cyclohexane ethylacetate溶媒

実験手順

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 liters 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).

後処理

  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

出典と根拠

ORDレコード
ord-c58f3ff2753a4d5aad828e6b8423bd4a
出典データセット
uspto-grants-2003_05
特許番号
US06563008B2

関連ノート

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