Sodium Carbonate → HCID 178422452, 화합물

HRID 1921800노트

반응식

HRID 1921800 반응식
[CH3:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4](O)[CH:3]=1.P(Br)(Br)([Br:12])=O.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.O>[Br:12][C:4]1[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]([OH:8])[CH:5]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 24613Phosphorus oxybromideHCID 178429093HCID 178429093, 화합물

생성물 1

HCID 178422452HCID 178422452, 화합물수율 46.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

A solution of 6-methylpyridine-2,4-diol (1.75 g, 14.0 mmol) in dry DMF (6.0 mL) is stirred under N2 and phosphorus oxybromide (3.05 g, 10.6 mmol) is added in one portion. The mixture is heated at 110° C. for 45 min and then cooled and diluted with water (7 mL). Na2CO3 (s) is added to bring the pH to 7 and the resulting suspension is cooled to 0° C. The product is collected by suction filtration, rinsing with cold water and diethyl ether, and dried overnight in a vacuum desiccator to afford the title compound as a light brown solid (920 mg).

후처리

  1. temperaturecooled
  2. temperaturethe resulting suspension is cooled to 0° C
  3. filtrationThe product is collected by suction filtration
  4. washrinsing with cold water and diethyl ether
  5. customdried overnight in a vacuum desiccator

출처 및 근거

ORD 기록
ord-d9ea4a56ad994373bcad63070090616e
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173656B2

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