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

HRID 1598569노트

반응식

HRID 1598569 반응식
[CH2:1]([S:5]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH2:19][CH2:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1)(=[O:7])=[O:6])[CH2:2][CH2:3][CH3:4].[OH-].[Na+].[N+](C1C=C(S([O-])(=O)=O)C=CC=1)([O-])=O.[Na+].Cl>O>[CH2:1]([S:5]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1)(=[O:6])=[O:7])[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 31389Sodium 3-nitrobenzenesulfonateHCID 189297852-n-butylsulfonylamino-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane

생성물 1

HCID 189298022-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane수율 66.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In 55 ml of water were dissolved 2.45 g of 2-n-butylsulfonylamino-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane and 1.40 g of sodium hydroxide, and 2.66 g of sodium 3-nitrobenzenesulfonate was added thereto. The mixture was refluxed under heating for 5 hours. After cooling, the reaction mixture was made acidic with 10% hydrochloric acid and extracted with ethyl acetate, the extract was dried, and then the solvent was removed. The resulting crystals were recrystallized from methanol to obtain 1.62 g of 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]-indane.

후처리

  1. additionwas added
  2. temperatureThe mixture was refluxed
  3. temperatureunder heating for 5 hours
  4. temperatureAfter cooling
  5. extractionextracted with ethyl acetate
  6. customthe extract was dried
  7. customthe solvent was removed
  8. customThe resulting crystals were recrystallized from methanol

출처 및 근거

ORD 기록
ord-3c945ea507404257b2fb5ee33d929fd4
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739132

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