1,1'-Carbonyldiimidazole → 3-[3-(4-pyridylthio)propyl]quinazoline-2,4(1H,3H)-dione

HRID 274719

반응식

HRID 274719 반응식
[NH2:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][S:10][C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1)=[O:5].[C:21](N1C=CN=C1)(N1C=CN=C1)=[O:22]>O1CCCC1>[N:14]1[CH:15]=[CH:16][C:11]([S:10][CH2:9][CH2:8][CH2:7][N:6]2[C:4](=[O:5])[C:3]3[C:2](=[CH:20][CH:19]=[CH:18][CH:17]=3)[NH:1][C:21]2=[O:22])=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 190790734-[3-(2-Aminobenzoylamino)propylthio]pyridine

생성물 1

HCID 190790923-[3-(4-pyridylthio)propyl]quinazoline-2,4(1H,3H)-dione수율 65.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Under nitrogen atmosphere, to a solution of 718 mg (2.5 mmol) of 4-[3-(2-aminobenzoylamino)propylthio]pyridine in 15 ml of tetrahydrofuran, 811 mg (5.0 mmol) of 1,1'-carbonyldiimidazole was added, and the mixture was stirred at room temperature for 16 hours. The solvent was distilled off and the residue was dissolved in chloroform. The solution was washed with water and dried. The solvent was distilled off and the residue was recrystallized from ethanol/chloroform/ether to give 514 mg of the desired product (65.7% yield, white crystals).

후처리

  1. distillationThe solvent was distilled off
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe solution was washed with water
  4. customdried
  5. distillationThe solvent was distilled off
  6. customthe residue was recrystallized from ethanol/chloroform/ether

출처 및 근거

ORD 기록
ord-80cfdf591e994b31a0bd71ca1fd94714
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389658

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