Hydrogen Bromide → 5-(Bromomethyl)-1H-indazole--hydrogen bromide (1/1)

HRID 1263432ノート

反応式

HRID 1263432 の反応式
C([N:4]1[C:12]2[C:7](=[CH:8][C:9]([CH2:13]OC(=O)C)=[CH:10][CH:11]=2)[CH:6]=[N:5]1)(=O)C.[BrH:18]>>[BrH:18].[Br:18][CH2:13][C:9]1[CH:8]=[C:7]2[C:12](=[CH:11][CH:10]=1)[NH:4][N:5]=[CH:6]2

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 107995691-Acetyl-5-(acetoxymethyl)indazole

生成物 1

HCID 226614415-(Bromomethyl)-1H-indazole--hydrogen bromide (1/1)

実験手順

A suspension of 1-acetyl-5-(acetoxymethyl)indazole (91) (3.0 g, 13 mmol) in aqueous hydrobromic acid (15 mL, 226 mmol) was stirred at room temperature for 25 hours. The solid was collected on a Buchner funnel and dried under vacuum for 12 hours. The filtrate was stirred at room temperature for additional 24 hours and more solid was collected. After drying under vacuum, title compound was obtained as a yellow solid (92, 3.48 g, 92%) which was used in the next synthesis step without further purification. 1H NMR (CDCl3) δ4.88 (s, 2H), 7.43 (d, 1H, J=8.8), 7.56 (d, 1H, J=8.8 Hz), 7.87 (s, 1H), 8.10 (s, 1H).

後処理

  1. customThe solid was collected on a Buchner funnel
  2. customdried under vacuum for 12 hours
  3. stirringThe filtrate was stirred at room temperature for additional 24 hours
  4. custommore solid was collected
  5. customAfter drying under vacuum

出典と根拠

ORDレコード
ord-3c29e5abe8b24e56b1883ba7edc488d3
出典データセット
uspto-grants-2003_04
特許番号
US06541467B1

反応ノート

読み込み中…