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Potassium Carbonate → HCID 86723024、化合物

HRID 522311
ノート
印刷プレビュー

反応式

HRID 522311 の反応式
Br[CH:2]1[CH2:8][CH2:7][CH2:6][CH2:5][O:4][C:3]1=[O:9].[Cl:10][C:11]1[C:12]([C:17]([F:20])([F:19])[F:18])=[N:13][NH:14][C:15]=1[CH3:16].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:10][C:11]1[C:12]([C:17]([F:19])([F:18])[F:20])=[N:13][N:14]([CH:2]2[CH2:8][CH2:7][CH2:6][CH2:5][O:4][C:3]2=[O:9])[C:15]=1[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12069654-Chloro-5-methyl-3-(trifluoromethyl)-1H-pyrazoleHCID 10954409HCID 10954409、化合物

生成物 1

HCID 86723024HCID 86723024、化合物収率 20%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
65 °C

実験手順

To a solution of 3-bromooxepan-2-one (1 g, 5.18 mmol) in DMF (10 mL) was added 4-chloro-5-methyl-3-(trifluoromethyl)-1H-pyrazole (0.956 g, 5.18 mmol), followed by potassium carbonate (1.07 g, 7.74 mmol). The reaction mixture was then heated at 65° C. for 8 h. After cooling to room temperature, the reaction mixture was partitioned between water (20 mL) and ethyl acetate (30 mL). The organic layers were washed with water and brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography (SiO2, 25% EtOAc/hexanes) gave the title product as a white solid (0.3 g, 1.01 mmol, 20%).

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe reaction mixture was partitioned between water (20 mL) and ethyl acetate (30 mL)
  3. washThe organic layers were washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customPurification by flash chromatography (SiO2, 25% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-97e28a6608b441cca0be87cef814a802
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328116B2

反応ノート

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