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

HRID 1598567

反応式

HRID 1598567 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5af222c59385436a96b3c24993006ea6
出典データセット
uspto-grants-1998_04
特許番号
US05739132

関連ノート

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