Water → 4-Bromo-6-methylpyridin-2-ol

HRID 252357ノート

反応式

HRID 252357 の反応式
P(Br)(Br)([Br:3])=O.O[C:7]1[CH:12]=[C:11]([CH3:13])[NH:10][C:9](=[O:14])[CH:8]=1.O.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[Br:3][C:7]1[CH:12]=[C:11]([CH3:13])[NH:10][C:9](=[O:14])[CH:8]=1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 24613Phosphorus oxybromideHCID 546914196-Methylpyridine-2,4-diol

生成物 1

HCID 231494724-Bromo-6-methylpyridin-2-ol

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

16 mmol of phosphorus oxybromide are added under an argon atmosphere to a solution of 21 mmol of 4-hydroxy-6-methyl-1H-pyridin-2-one [3749-51-7] in 9 ml of N,N-dimethylformamide. The reaction mixture is heated to 110° C. for 30 minutes and subsequently cooled to room temperature, and 10 ml of water are added. The solution is brought to pH 7 by adding sodium carbonate and cooled to 0° C. The precipitate is filtered off and washed with water and diethyl ether. The title compound is identified on the basis of the Rf value.

後処理

  1. temperaturesubsequently cooled to room temperature
  2. temperaturecooled to 0° C
  3. filtrationThe precipitate is filtered off
  4. washwashed with water and diethyl ether

出典と根拠

ORDレコード
ord-4df7562c70004bd9a4222574ff17c932
出典データセット
uspto-grants-2011_01
特許番号
US07868036B2

反応ノート

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