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

HRID 6180ノート

反応式

HRID 6180 の反応式
[NH2:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][S:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1)=[O:5].[C:22](N1C=CN=C1)(N1C=CN=C1)=[O:23]>O1CCCC1>[N:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[S:11][CH2:10][CH2:9][CH2:8][CH2:7][N:6]1[C:4](=[O:5])[C:3]2[C:2](=[CH:21][CH:20]=[CH:19][CH:18]=2)[NH:1][C:22]1=[O:23]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 19079132HCID 19079132、化合物

生成物 1

HCID 190791813-[4-(2-pyridylthio)butyl]quinazoline-2,4(1H,3H)-dione収率 68.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under nitrogen atmosphere, to a solution of 452 mg (1.5 mmol) of 2-[4-(2-aminobenzoylamino)butylthio]pyridine in 20 ml of tetrahydrofuran, 486 mg (3.0 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 chloroform/ether to give 337 mg of the desired product (68.8% yield, white crystals).

後処理

  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 chloroform/ether

出典と根拠

ORDレコード
ord-32b0f994e35548499b85f980112ef12f
出典データセット
uspto-grants-1993_09
特許番号
US05246948

反応ノート

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