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

HRID 488813

반응식

HRID 488813 반응식
[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

참가 물질

4

반응물 2

HCID 142752-Methyl-5-hydroxypyridineHCID 24408Bromine

생성물 1

HCID 119591012-Bromo-6-methylpyridin-3-ol수율 53.1%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-09e18de15b464aafb3daf4cb88714ba4
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06974826B2

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