Benzenesulfonyl chloride → HCID 18929758、化合物

HRID 1598578ノート

反応式

HRID 1598578 の反応式
I.[N:2]1[NH:3][C:4](=[O:18])[CH2:5][CH2:6][C:7]=1[C:8]1[S:12][C:11]2[CH2:13][CH2:14][CH:15]([NH2:17])[CH2:16][C:10]=2[CH:9]=1.C(N(CC)CC)C.[C:26]1([S:32](Cl)(=[O:34])=[O:33])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>CN1CCN(C)C1=O>[N:2]1[NH:3][C:4](=[O:18])[CH2:5][CH2:6][C:7]=1[C:8]1[S:12][C:11]2[CH2:13][CH2:14][CH:15]([NH:17][S:32]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)(=[O:34])=[O:33])[CH2:16][C:10]=2[CH:9]=1

参加物

5

反応物 3

HCID 7369Benzenesulfonyl chlorideHCID 8471TriethylamineHCID 18929750HCID 18929750、化合物

生成物 1

HCID 18929758HCID 18929758、化合物収率 88.2%

試薬・触媒・溶媒 1

HCID 66611,3-Dimethyl-2-imidazolidinone溶媒

実験手順

To 1.34 g of 2-[4,5-dihydropyridazin-3(2H)-on-6-yl]-5-amino-4,5,6,7-tetrahydrobenzo[b]thiophene.hydroiodide and 1.2 ml of triethylamine dissolved in 20 ml of 1,3-dimethyl-2-imidazolidinone was added 765 mg of benzenesulfonyl chloride, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into ice water and extracted with ethyl acetate. After the organic layer was washed and dried, the solvent was removed. The resulting crystals were recrystallized from nitromethane to obtain 1.22 g of 2-[4,5-dihydropyridazin-3(2H)-on-6-yl]-5-(phenylsulfonylamino)-4,5,6,7-tetrahydrobenzo[b]thiophene.

後処理

  1. extractionextracted with ethyl acetate
  2. washAfter the organic layer was washed
  3. customdried
  4. customthe solvent was removed
  5. customThe resulting crystals were recrystallized from nitromethane

出典と根拠

ORDレコード
ord-dba9202ba71f40febfc52f262d392cf8
出典データセット
uspto-grants-1998_04
特許番号
US05739132

反応ノート

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