Benzyl Bromide → HCID 22711808、化合物

HRID 1359272

反応式

HRID 1359272 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 22711808HCID 22711808、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9428576bcc0e46c2af241a37be4cb3bb
出典データセット
uspto-grants-2003_07
特許番号
US06599917B1

関連ノート

読み込み中…