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 1378533노트

반응식

HRID 1378533 반응식
[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

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a42f888951b4be6b000aa1c5a464879
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05668152

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