Acetic Acid → (1-phenyl-1H-pyrazol-5-yl)boronic acid

HRID 333721

反応式

HRID 333721 の反応式
[C:1]1([N:7]2[CH:11]=[CH:10][CH:9]=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([Li])CCC.[B:17](OC(C)C)([O:22]C(C)C)[O:18]C(C)C.C(O)(=O)C>O1CCCC1>[C:1]1([N:7]2[C:11]([B:17]([OH:22])[OH:18])=[CH:10][CH:9]=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

実験手順

To a solution of 1-phenyl-1H-pyrazole (20.0 g) in tetrahydrofuran (700 mL) was added dropwise n-butyllithium (2.5M hexane solution, 58.3 mL) under a nitrogen atmosphere at −78° C., and the mixture was stirred at the same temperature for min. To the reaction mixture was added triisopropyl borate (52.2 g) at −78° C., and the mixture was stirred at the same temperature for 1 hr. The mixture was gradually warmed to room temperature, and stirred at room temperature for 20 hr. To the reaction mixture was added acetic acid (20 mL) to adjust to pH 5, and the mixture was concentrated to give the title compound (25.0 g).

後処理

  1. stirringthe mixture was stirred at the same temperature for 1 hr
  2. stirringstirred at room temperature for 20 hr
  3. concentrationthe mixture was concentrated

出典と根拠

ORDレコード
ord-0ce174f833cc450e97e671a0493ec689
出典データセット
uspto-grants-2014_11
特許番号
US08883788B2

関連ノート

読み込み中…