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Imidazole → HCID 85051032、化合物

HRID 2179912
ノート
印刷プレビュー

反応式

HRID 2179912 の反応式
[C:1]([Si:5](Cl)([CH3:7])[CH3:6])([CH3:4])([CH3:3])[CH3:2].[CH3:9][N:10]([CH3:32])[CH:11]1[C:25]2=[CH:26][CH:22]([O:23][C:24]2=[O:27])[CH:21]2[CH:17]([O:18][C:19](=[O:29])[CH:20]2[CH3:28])[CH2:16][C:15]2([CH3:30])[CH:13]([O:14]2)[CH:12]1[OH:31].N1C=CN=C1.O>CN(C=O)C>[O:31]([CH:12]1[CH:11]([N:10]([CH3:9])[CH3:32])[C:25]2=[CH:26][CH:22]([O:23][C:24]2=[O:27])[CH:21]2[CH:17]([O:18][C:19](=[O:29])[CH:20]2[CH3:28])[CH2:16][C:15]2([CH3:30])[CH:13]1[O:14]2)[Si:5]([C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:7])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 86592994HCID 86592994、化合物

生成物 1

HCID 85051032HCID 85051032、化合物収率 55.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Terbutyldimethylsilyl chloride (80 μmol, 12 mg) is added to a solution of the compound of Example 5 (80 μmol; 27 mg) and imidazole (160 μmol; 11 mg) in DMF (0.5 ml). The solution obtained is stirred for 20 hours then the reaction mass is poured into water. The aqueous phase is extracted twice with ethyl acetate, the organic phase is washed with water then with a solution of sodium chloride. The organic phase is dried over magnesium sulphate, filtered then evaporated. The residue is eluted on silica with a mixture of isopropyl acetate and dichloromethane (20/80). 20 mg of product is obtained in the form of a white powder.

後処理

  1. customThe solution obtained
  2. extractionThe aqueous phase is extracted twice with ethyl acetate
  3. washthe organic phase is washed with water
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. filtrationfiltered
  6. customthen evaporated
  7. washThe residue is eluted on silica with a mixture of isopropyl acetate and dichloromethane (20/80)

出典と根拠

ORDレコード
ord-48e14922316344b3a384cf25794cfdfe
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06887869B2

反応ノート

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