Benzenesulfonyl chloride → HCID 18929758, 화합물

HRID 1598578노트

반응식

HRID 1598578 반응식
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

참가 물질

5

반응물 3

HCID 7369Benzenesulfonyl chlorideHCID 8471TriethylamineHCID 18929750HCID 18929750, 화합물

생성물 1

HCID 18929758HCID 18929758, 화합물수율 88.2%

시약·촉매·용매 1

HCID 66611,3-Dimethyl-2-imidazolidinone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dba9202ba71f40febfc52f262d392cf8
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739132

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