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

HRID 2293100ノート

反応式

HRID 2293100 の反応式
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]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 7914Diisopropyl EtherHCID 21476308HCID 21476308、化合物HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-027cb871a4a2459f964b157995424a9c
出典データセット
uspto-grants-1997_11
特許番号
US05686452

反応ノート

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