Imidazole → 4-{[tert-Butyl(dimethyl)silyl]oxy}-1H-pyrazole

HRID 1003798ノート

反応式

HRID 1003798 の反応式
[OH:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.N1C=CN=C1.[Si:12](Cl)([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13]>CN(C=O)C>[Si:12]([O:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1)([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13]

参加物

5

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 1192181H-Pyrazol-4-ol

生成物 1

HCID 206558384-{[tert-Butyl(dimethyl)silyl]oxy}-1H-pyrazole収率 94.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Hydroxypyrazole (1.16 g, 13.8 mmol) and imidazole (1.13 g, 16.6 mmol) were suspended in DMF (50 ml) under nitrogen and t-butyldimethylsilylchloride (2.3 g, 15.2 mmol) was added. After stirring 17 hours, the solvent was removed in vacuo and the residue treated with water containing 4.5 g of potassium carbonate. The mixture was extracted with two portions of chloroform and the organic layer dried over sodium sulfate. The solvent was removed in vacuo to yield product (2.58 g, 94%). NMR

後処理

  1. customthe solvent was removed in vacuo
  2. additionthe residue treated with water containing 4.5 g of potassium carbonate
  3. extractionThe mixture was extracted with two portions of chloroform
  4. dry with materialthe organic layer dried over sodium sulfate
  5. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-2ae8c3751f4b427cbed14871ef047000
出典データセット
uspto-grants-2000_04
特許番号
US06046227

反応ノート

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