Bromine → HCID 178478419, 화합물

HRID 268869

반응식

HRID 268869 반응식
[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]

참가 물질

5

반응물 2

HCID 24408BromineHCID 958943-Chloro-1H-indazole

생성물 1

HCID 178478419HCID 178478419, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7e4ebfc6579e44509b9a6fc46fe0eaf7
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07446118B2

연결된 노트

불러오는 중…