Bromine → HCID 178478419、化合物

HRID 268869

反応式

HRID 268869 の反応式
[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][N:3]=1.[Br:11]Br>CC(O)=O.CCOC(C)=O>[Br:11][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[NH:4][N:3]=[C:2]2[Cl:1]

参加物

5

反応物 2

HCID 24408BromineHCID 958943-Chloro-1H-indazole

生成物 1

HCID 178478419HCID 178478419、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a room temperature solution of 3-chloro-1H-indazole (10.0 g, 65.5 mmol) in AcOH (250 ml) was added Br2 (3.54 ml, 68.8 mmol) dropwise. The reaction mixture was stirred at room temperature for 18 hours, then diluted with EtOAc (500 ml), washed with aqueous NaOH solution (10%), saturated aqueous NaHCO3 and brine. The organic layer was dried over MgSO4, filtered, concentrated, and the residue was recrystallized from toluene. The solid was washed with hexanes and dried in vacuo affording 5-Bromo-3-chloro-1H-indazole CCXIV as a white solid (54% yield).

後処理

  1. washwashed with aqueous NaOH solution (10%), saturated aqueous NaHCO3 and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customthe residue was recrystallized from toluene
  6. washThe solid was washed with hexanes
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-7e4ebfc6579e44509b9a6fc46fe0eaf7
出典データセット
uspto-grants-2008_11
特許番号
US07446118B2

関連ノート

読み込み中…