Hydrochloric Acid → 3-[1-(1-Methyl-piperidin-4-yl)-indol-3-yl]-4-(1-methyl-indol-3-yl)-1H-pyrrole-2,5-dione hydrochloride

HRID 1077949ノート

反応式

HRID 1077949 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([C:17]3[C:18](=[O:33])[NH:19][C:20](=[O:32])[C:21]=3[C:22]3[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[N:24]([CH3:31])[CH:23]=3)=[CH:9]2)[CH2:4][CH2:3]1.[ClH:34]>C(OCC)(=O)C.CO>[ClH:34].[CH3:1][N:2]1[CH2:3][CH2:4][CH:5]([N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([C:17]3[C:18](=[O:33])[NH:19][C:20](=[O:32])[C:21]=3[C:22]3[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[N:24]([CH3:31])[CH:23]=3)=[CH:9]2)[CH2:6][CH2:7]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 98893513-[1-(1-Methyl-piperidin-4-yl)-indol-3-yl]-4-(1-methyl-indol-3-yl)-1H-pyrrole-2,5-dione

生成物 1

HCID 229072523-[1-(1-Methyl-piperidin-4-yl)-indol-3-yl]-4-(1-methyl-indol-3-yl)-1H-pyrrole-2,5-dione hydrochloride

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

An ice cooled solution of 3-[1-(1-methyl-piperidin-4-yl)-1H-indol-3-yl]-4-(1-methyl-1H-indol-3-yl)-pyrrole-2,5-dione (70 g, 0.16 mol) in ethyl acetate (4 L) was saturated with gaseous hydrogen chloride for 3 hours. The precipitate formed was isolated by suction filtration, suspended in methanol (3 L) and stirred for 30 minutes. The mixture turned into a homogenous slurry, which was concentrated and treated with ether (500 mL). The title compound crystallized and was collected by suction filtration. The filter was vacuum dried over night (100° C./0.1 mm. Yield 70 g (92% of theory). M.Pt.: 280°-282° C.

後処理

  1. customThe precipitate formed
  2. customwas isolated by suction filtration
  3. concentrationwas concentrated
  4. additiontreated with ether (500 mL)
  5. customThe title compound crystallized
  6. filtrationwas collected by suction filtration
  7. customdried over night (100° C./0.1 mm

出典と根拠

ORDレコード
ord-01bbb547490a43d991aa3779a8b67471
出典データセット
uspto-grants-1996_08
特許番号
US05545636

反応ノート

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