Triethylamine → HCID 21476308、化合物

HRID 2293105ノート

反応式

HRID 2293105 の反応式
C(N(CC)CC)C.[NH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1.[CH2:26]([S:29](Cl)(=[O:31])=[O:30])[CH2:27][CH3:28]>CN1CCN(C)C1=O.O1CCCC1>[CH2:26]([S:29]([NH:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1)(=[O:31])=[O:30])[CH2:27][CH3:28]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 21476304HCID 21476304、化合物

生成物 1

HCID 21476308HCID 21476308、化合物収率 61.7%

試薬・触媒・溶媒 2

HCID 66611,3-Dimethyl-2-imidazolidinone溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5.53 g of triethylamine was added to 6.03 g of 2-aminomethyl-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane suspended in 60 ml of 1,3-dimethyl-2-imidazolidinone, and then 5.10 g of propanesulfonyl chloride dissolved in 20 ml of tetrahydrofuran was added to the mixture. The resulting mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into ice water, and crystals precipitated were collected by filtration. The precipitated crystals were recrystallized from methanol-acetonitrile to obtain 5.34 g of 2-(propylsulfonylaminomethyl)-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane

後処理

  1. additionwas added to the mixture
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. customThe precipitated crystals were recrystallized from methanol-acetonitrile

出典と根拠

ORDレコード
ord-d04d03f739b44764a609e864c48331e4
出典データセット
uspto-grants-1997_11
特許番号
US05686452

反応ノート

読み込み中…