Dimethyl Sulfoxide → 2-(propylsulfonylaminomethyl)-5-[pyridazin-3(2H)-on-6-yl]indane

HRID 2293100노트

반응식

HRID 2293100 반응식
Br.C(O)(=O)C.CS(C)=O.[CH2:10]([S:13]([NH:16][CH2:17][CH:18]1[CH2:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([C:27]3[CH2:28][CH2:29][C:30](=[O:33])[NH:31][N:32]=3)[CH:24]=2)[CH2:19]1)(=[O:15])=[O:14])[CH2:11][CH3:12].C(OC(C)C)(C)C>C(O)(=O)C>[CH2:10]([S:13]([NH:16][CH2:17][CH:18]1[CH2:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([C:27]3[CH:28]=[CH:29][C:30](=[O:33])[NH:31][N:32]=3)[CH:24]=2)[CH2:19]1)(=[O:15])=[O:14])[CH2:11][CH3:12]

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 7914Diisopropyl EtherHCID 21476308HCID 21476308, 화합물HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 214763052-(propylsulfonylaminomethyl)-5-[pyridazin-3(2H)-on-6-yl]indane수율 92.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

25 ml of 30% hydrogen bromide-acetic acid and 1.3 ml of dimethyl sulfoxide were added to 5.24 g of 2-(propylsulfonylaminomethyl)-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane suspended in 60 ml of acetic acid. The mixture was stirred at room temperature for 2 hours. 150 ml of isopropyl ether was added to the mixture, and crystals precipitated were collected by filtration, washed with water, dried and then recrystallized from methanol to obtain 4.82 g of 2-(propylsulfonylaminomethyl)-5-[pyridazin-3(2H)-on-6-yl]indane. This compound had the same physical properties as those of the compound obtained in Example 2.

후처리

  1. customprecipitated
  2. filtrationwere collected by filtration
  3. washwashed with water
  4. customdried
  5. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-027cb871a4a2459f964b157995424a9c
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686452

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