Sodium Carbonate → HCID 10731614, 화합물

HRID 580922

반응식

HRID 580922 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 10731614HCID 10731614, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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.).

후처리

  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.)

출처 및 근거

ORD 기록
ord-d1941fde172f477b96484c5054a58e59
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919799

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