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

HRID 400241

反応式

HRID 400241 の反応式
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[C:3]([Br:8])[CH:2]=1.CN(C)C=O.N1C=CN=C1.[CH3:19][C:20]([Si:23]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)Cl)([CH3:22])[CH3:21]>O>[Br:8][C:3]1[CH:4]=[CH:5][C:6]([O:7][Si:23]([C:20]([CH3:22])([CH3:21])[CH3:19])([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:1][CH:2]=1

参加物

6

反応物 4

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

生成物 1

HCID 11292808Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl-収率 95.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

80.89 g of p-bromophenol, 400 ml of dimethylformamide, 31.18 g of imidazole and 125.89 g of 1,1-dimethyl-ethyl-diphenylchlorosilane were stirred for 2 hours at ambient temperature and the reaction medium was poured into 2 liters of water. Extraction was carried out with ethyl acetate, followed by decanting, drying and evaporating under reduced pressure. After crystallization from pentane, separation was carried out, followed by drying to obtain 179.24 g of the expected product with a Rf=0.53 (thin layer chromatography, support: silica, eluant: cyclohexane/AcOEt 95/5) and a melting point of 56° C.

後処理

  1. extractionExtraction
  2. customby decanting
  3. customdrying
  4. customevaporating under reduced pressure
  5. customAfter crystallization
  6. customfrom pentane, separation
  7. customby drying

出典と根拠

ORDレコード
ord-8854cb3665544fa08f3b945a9648e0a4
出典データセット
uspto-grants-1998_10
特許番号
US05827887

関連ノート

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