2-Methyl-5-hydroxypyridine → 2-Bromo-6-methylpyridin-3-ol

HRID 488813

反応式

HRID 488813 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.[Br:9]Br>N1C=CC=CC=1>[Br:9][C:7]1[C:2]([OH:1])=[CH:3][CH:4]=[C:5]([CH3:8])[N:6]=1

参加物

4

反応物 2

HCID 142752-Methyl-5-hydroxypyridineHCID 24408Bromine

生成物 1

HCID 119591012-Bromo-6-methylpyridin-3-ol収率 53.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

To a solution of 5-hydroxy-2-methylpyridine (8.80 g, 80.6 mmol) in 125 mL of pyridine was added a solution of bromine (14.18 g, 88.7 mmol) in 50 mL pyridine dropwise. The temperature of the reaction mixture rose to 40° C. upon completion of addition. After 1 hour the pyridine was removed under vacuum and the resulting solid was suspended into water (200 mL) and stirred overnight. The solid was collected and dried to give the desire product as a brownish solid (8.05 g, 53.1% yield). 1H NMR (500 MHz, CDCl3): δ 2.21 (s, 3 H), 6.73 (d, J=8.1 Hz, 1 H), 6.94 (d, J=8.1 Hz, 1 H), 9.36 (brs, 1 H).

後処理

  1. additionThe temperature of the reaction mixture rose to 40° C. upon completion of addition
  2. customAfter 1 hour the pyridine was removed under vacuum
  3. customThe solid was collected
  4. customdried

出典と根拠

ORDレコード
ord-09e18de15b464aafb3daf4cb88714ba4
出典データセット
uspto-grants-2005_12
特許番号
US06974826B2

関連ノート

読み込み中…