Bromine → 4-(4-bromo-1H-pyrazol-1-yl)pyridine

HRID 2274761

反応式

HRID 2274761 の反応式
[N:1]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=2)[CH:5]=[CH:4][CH:3]=[N:2]1.[Br:12]Br>C(O)(=O)C.[O-]S([O-])(=S)=O.[Na+].[Na+]>[Br:12][C:4]1[CH:3]=[N:2][N:1]([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=2)[CH:5]=1

参加物

5

反応物 2

HCID 24408BromineHCID 200417044-(1H-Pyrazol-1-yl)pyridine2 回

生成物 1

HCID 545954894-(4-bromo-1H-pyrazol-1-yl)pyridine収率 55%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 24477Sodium Thiosulfate溶媒

実験手順

To a solution of 4-(1H-pyrazol-1-yl)pyridine (Intermediate 7; 1.1 g; 7.5 mmol) in acetic acid (10 mL) was added a solution of bromine (6 mL) in acetic acid (10 mL) dropwise. The reaction mixture was stirred for 4 hours, diluted with saturated aqueous Na2S2O3 (20 mL), and extracted with DCM (10 mL×3). The combined organic layers were washed with saturated aqueous NaHCO3 (20 mL), water (20 mL), brine (20 mL), dried over anhydrous Na2SO4, filtered, and concentrated to afford 936 mg (55%) of the title compound as a pink solid.

後処理

  1. extractionextracted with DCM (10 mL×3)
  2. washThe combined organic layers were washed with saturated aqueous NaHCO3 (20 mL), water (20 mL), brine (20 mL)
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-17a3d2aa27e4443195c3eaf9e5d7dde5
出典データセット
uspto-grants-2015_09
特許番号
US09126984B2

関連ノート

読み込み中…