Sodium Carbonate → HCID 10731614、化合物

HRID 580922

反応式

HRID 580922 の反応式
[C:1]1([C:7]2[N:8]=[C:9]3[N:13]([CH:14]=2)[C:12]2[CH2:15][CH2:16][CH2:17][CH2:18][C:11]=2[S:10]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)=O.[C:24](=O)([O-])[O-:25].[Na+].[Na+]>CN(C)C=O>[C:1]1([C:7]2[N:8]=[C:9]3[N:13]([C:14]=2[CH:24]=[O:25])[C:12]2[CH2:15][CH2:16][CH2:17][CH2:18][C:11]=2[S:10]3)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 7608862-Phenyl-5,6,7,8-tetrahydroimidazo[2,1-b][1,3]benzothiazole

生成物 1

HCID 10731614HCID 10731614、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

3.35 g of 5,6,7,8-tetrahydro-2-phenylimidazo[2,1-b]benzothiazole was suspended in 20 ml of dimethylformamide. To the resultant mixture, 3 ml of phosphorus oxychloride was added dropwise at 0° C. over 10 minutes. The solution was gradually returned to room temperature, then heated and stirred at 60° C. for 3 hours, poured onto an aqueous sodium carbonate solution, then extracted with chloroform. The solvent was distilled off, the residue was then recrystallized from ethanol to obtain the desired substance in an amount of 2.31 g (yield of 82.0%) (melting point:150-150.5° C.).

後処理

  1. customwas gradually returned to room temperature
  2. temperatureheated
  3. extractionextracted with chloroform
  4. distillationThe solvent was distilled off
  5. customthe residue was then recrystallized from ethanol
  6. customto obtain the desired substance in an amount of 2.31 g (yield of 82.0%) (melting point:150-150.5° C.)

出典と根拠

ORDレコード
ord-d1941fde172f477b96484c5054a58e59
出典データセット
uspto-grants-1999_07
特許番号
US05919799

関連ノート

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