Sodium hydride → 2-(3,4-Dimethoxyphenyl)-4-(4-methylpiperazinylmethyl)thiazole

HRID 1489249

反応式

HRID 1489249 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([CH2:16]Cl)[N:15]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.[H-].[Na+]>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([CH2:16][N:22]3[CH2:23][CH2:24][N:19]([CH3:18])[CH2:20][CH2:21]3)[N:15]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 531671-MethylpiperazineHCID 20793964-(Chloromethyl)-2-(3,4-dimethoxyphenyl)-1,3-thiazole

生成物 1

HCID 187072282-(3,4-Dimethoxyphenyl)-4-(4-methylpiperazinylmethyl)thiazole収率 77.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 10 ml of dimethylformamide were dissolved 860 mg of 2-(3,4-dimethoxyphenyl)-4-chloromethylthiazole and 320 mg of N-methylpiperazine. Thereto was added 130 mg of sodium hydride. The mixture was stirred at room temperature for 14 hours. The solvent was removed by distillation. The residue was extracted with chloroform. The extract was water-washed, dried and subjected to distillation to remove the solvent. The residue was dissolved in ethanol. To the solution was added ethanol saturated with hydrogen chloride gas, and the mixture was allowed to stand. The resulting crystals were collected by filtration, washed with a small amount of ethanol, dried and recrystallized from ethanol to obtain 820 mg of 2-(3,4-dimethoxyphenyl)-4-(4-methylpiperazinylmethyl)thiazole.

後処理

  1. customThe solvent was removed by distillation
  2. extractionThe residue was extracted with chloroform
  3. washwashed
  4. customdried
  5. distillationsubjected to distillation
  6. customto remove the solvent
  7. dissolutionThe residue was dissolved in ethanol
  8. additionTo the solution was added ethanol saturated with hydrogen chloride gas
  9. filtrationThe resulting crystals were collected by filtration
  10. washwashed with a small amount of ethanol
  11. customdried
  12. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-dff9a24000a744959b53632fef33dbc4
出典データセット
uspto-grants-1997_10
特許番号
US05677319

関連ノート

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