Hydrogen iodide → 6-hydroxy-1H-indazole

HRID 1750114

反応式

HRID 1750114 の反応式
C[O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH:7]=[N:8][NH:9]2)=[CH:5][CH:4]=1.I>>[NH:9]1[C:10]2[C:6](=[CH:5][CH:4]=[C:3]([OH:2])[CH:11]=2)[CH:7]=[N:8]1

参加物

3

反応物 2

HCID 24841Hydrogen iodideHCID 126392026-Methoxy-1H-indazole

生成物 1

HCID 1354839876-hydroxy-1H-indazole収率 86%

実験手順

A mixture of 6-methoxy-1H-indazole (560 mg, 3.8 mmol) and HI (2.4 mL 48%) was heated to reflux for 4 h. The mixture was extracted with CH2Cl2. The combined organic layers were washed with water, brine, concentrated in vacuo, and purified by column chromatography (CH2Cl2/MeOH=60/1) to give 1H-indazol-6-ol (intermediate 43) (436 mg, 86%).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4 h
  3. extractionThe mixture was extracted with CH2Cl2
  4. washThe combined organic layers were washed with water, brine
  5. concentrationconcentrated in vacuo
  6. custompurified by column chromatography (CH2Cl2/MeOH=60/1)

出典と根拠

ORDレコード
ord-bce95d5fbb24486a961c4d7923b9ac97
出典データセット
uspto-grants-2015_10
特許番号
US09156822B2

関連ノート

読み込み中…