Triethylamine → 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane

HRID 1598567

반응식

HRID 1598567 반응식
[NH2:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:11]3[CH:12]=[CH:13][C:14](=[O:17])[NH:15][N:16]=3)[CH:8]=2)[CH2:3]1.C(N(CC)CC)C.[CH2:25]([S:29](Cl)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]>CN(C)C=O>[CH2:25]([S:29]([NH:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:11]3[CH:12]=[CH:13][C:14](=[O:17])[NH:15][N:16]=3)[CH:8]=2)[CH2:3]1)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 754301-Butanesulfonyl chlorideHCID 189297732-amino-5-[pyridazin-3(2H)-on-6-yl]indane

생성물 1

HCID 189298022-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane수율 72.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

In 50 ml of dimethylformamide were dissolved 1.14 g of 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane and 0.8 g of triethyl amine, and 1.25 g of n-butanesulfonyl chloride was added thereto. The mixture was stirred at 50° C for 30 minutes and then stirred at room temperature overnight. The solvent was removed, water was added to the residue, and crystals precipitated were collected by filtration. The resulting crystals were recrystallized from methanol to obtain 1.27 g of 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane.

후처리

  1. additionwas added
  2. stirringstirred at room temperature overnight
  3. customThe solvent was removed
  4. additionwater was added to the residue, and crystals
  5. customprecipitated
  6. filtrationwere collected by filtration
  7. customThe resulting crystals were recrystallized from methanol

출처 및 근거

ORD 기록
ord-5af222c59385436a96b3c24993006ea6
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739132

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