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Hydrochloric Acid → Bisindolylmaleimide XI hydrochloride

HRID 863670
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HRID 863670 반응식
FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.C(O[CH2:20][CH:21]1[CH2:50][CH2:49][N:24]2[C:25]3[C:30]([C:31]([C:32]4[C:33](=O)[O:34][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]2[CH2:22]1)=[CH:29][CH:28]=[CH:27][CH:26]=3)(=O)C.[N:51]1C(C)=CC(C)=CC=1C.[CH3:60][NH:61][CH3:62].[ClH:63]>ClCCl.C(O)C.C(OCC)(=O)C>[ClH:63].[CH3:60][N:61]([CH2:20][CH:21]1[CH2:50][CH2:49][N:24]2[C:25]3[C:30]([C:31]([C:32]4[C:33](=[O:34])[NH:51][C:35](=[O:47])[C:36]=4[C:37]4[C:45]5[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=5)[N:39]([CH3:46])[CH:38]=4)=[C:23]2[CH2:22]1)=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH3:62]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 79532,4,6-TrimethylpyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 103898823-[8-(Acetoxymethyl)-6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)furan-2,5-dione

생성물 1

HCID 11605551Bisindolylmaleimide XI hydrochloride

시약·촉매·용매 3

HCID 702Ethanol용매HCID 6344Dichloromethane용매2회HCID 8857Ethyl Acetate용매

실험 절차

185 mg of trifluoromethanesulfonic anhydride in 30 ml of dichloromethane were treated at 0° C. under a nitrogen atmosphere with a suspension of 140 mg of the pyrroledione product of Example 1 and 70 mg of collidine in 25 ml of dichloromethane. After 1.5 hour, 0.8 ml of a 33% solution of dimethylamine in ethanol was added and the mixture was stirred for 2.5 hours. The solvent was removed under reduced pressure and the residue was triturated with methanol to give a solid which was stirred with ethyl acetate saturated with hydrogen chloride. The solid was filtered off and dried to give 70 mg of 3-[6,7,8,9-tetrahydro-8-[(dimethylamino)methyl]pyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione hydrochloride of melting point 335°-336° C.

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was triturated with methanol
  3. customto give a solid which
  4. filtrationThe solid was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-b83a4150614b49c2b63fd84dfa1d1110
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05721245

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