Benzyl Bromide → HCID 22711808, 화합물

HRID 1359272

반응식

HRID 1359272 반응식
[OH:1][C:2]1[C:3]([CH2:9][OH:10])=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:17](Br)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CN(C)C=O>[CH2:17]([O:1][C:2]1[C:3]([CH2:9][OH:10])=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 1351283-Hydroxy-2-hydroxymethyl-6-methylpyridine

생성물 1

HCID 22711808HCID 22711808, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

100 g of 3-hydroxy-6-methyl-2-pyridine methanol and 150 g of potassium carbonate were suspended in 400 ml of N,N-dimethylformamide. Under heating under stirring 60° C. in an oil bath, 85 ml of benzyl bromide was added dropwise thereinto. Further, after heating under stirring for 30 minutes, insoluble matters were filtered off. Water was added to the filtrate, and the mixture was extracted with ethyl acetate. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was recrystallized from ethanol/hexane, to give 145 g of the target compound.

후처리

  1. temperatureUnder heating
  2. temperatureFurther, after heating
  3. stirringunder stirring for 30 minutes
  4. filtrationinsoluble matters were filtered off
  5. additionWater was added to the filtrate
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe organic phase was washed with water and brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. customThe residue was recrystallized from ethanol/hexane

출처 및 근거

ORD 기록
ord-9428576bcc0e46c2af241a37be4cb3bb
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06599917B1

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