Imidazole → HCID 54284754、化合物

HRID 2291292ノート

反応式

HRID 2291292 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].N1C=CN=C1.[C:16]1([Si:22](Cl)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:23]([CH3:26])([CH3:25])[CH3:24])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CN(C)C=O>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][Si:22]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:23]([CH3:26])([CH3:24])[CH3:25])=[O:6]

参加物

5

反応物 3

HCID 795ImidazoleHCID 74203-Hydroxybenzoic AcidHCID 94078tert-Butyldiphenylchlorosilane

生成物 1

HCID 54284754HCID 54284754、化合物収率 52.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To stirred solution of 50.4 g of 3-hydroxybenzoic acid in 200 ml of dry dimethylformamide at 0° C. was added 24.85 g of imidazole, followed by 100 g of diphenyl-(2-methylprop-2-yl)silyl chloride. The mixture was stirred at room temperature for 16 hours, and partitioned between ethyl acetate and cold water. The organic layer was washed with water, with an aqueous potassium hydrogen carbonate solution and with brine, was dried over anhydrous magnesium sulphate and evaporated to dryness. The resulting white solid was slurried in dry chloroform and filtered to afford 72 g of the title compound.

後処理

  1. custompartitioned between ethyl acetate and cold water
  2. washThe organic layer was washed with water, with an aqueous potassium hydrogen carbonate solution and with brine
  3. dry with materialwas dried over anhydrous magnesium sulphate
  4. customevaporated to dryness
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-9e8ffa4e6b3c4722a96061e80dbc1af1
出典データセット
uspto-grants-1989_01
特許番号
US04795748

反応ノート

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