Cesium carbonate → 4-Bromo-1-(oxetan-3-YL)-1H-pyrazole

HRID 515904노트

반응식

HRID 515904 반응식
[Br:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.Br[CH:8]1[CH2:11][O:10][CH2:9]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH:8]2[CH2:11][O:10][CH2:9]2)[CH:6]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 163754-BromopyrazoleHCID 162444933-Bromooxetane

생성물 1

HCID 739778714-Bromo-1-(oxetan-3-YL)-1H-pyrazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
130 °C

실험 절차

4-Bromo-1H-pyrazole (1.53 g, 10.7 mmol) is dissolved in anhydrous dimethylformamide (15 mL). 3-Bromooxetane (2.0 g, 14.6 mmol) and caesium carbonate (4.7 g, 14 mmol) are successively added thereto. The reaction mixture is heated for 8 hours at 130° C. in a sealed flask. At the end of the reaction, the solvent is evaporated off in vacuo and the residue is purified by chromatography over silica gel using dichloromethane containing diethylamine and methanol as eluants to yield the expected compound.

후처리

  1. customAt the end of the reaction
  2. customthe solvent is evaporated off in vacuo
  3. customthe residue is purified by chromatography over silica gel
  4. additioncontaining diethylamine and methanol as eluants

출처 및 근거

ORD 기록
ord-fc3f1cb3d3e44a0babd9c31d566c8cf5
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108983B2

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