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

HRID 1003798노트

반응식

HRID 1003798 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-2ae8c3751f4b427cbed14871ef047000
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06046227

반응 노트

불러오는 중…