Water → 4-Bromo-6-methylpyridin-2-ol

HRID 252357노트

반응식

HRID 252357 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4df7562c70004bd9a4222574ff17c932
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868036B2

반응 노트

불러오는 중…