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

HRID 515904ノート

反応式

HRID 515904 の反応式
[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

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 163754-BromopyrazoleHCID 162444933-Bromooxetane

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc3f1cb3d3e44a0babd9c31d566c8cf5
出典データセット
uspto-grants-2015_08
特許番号
US09108983B2

反応ノート

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