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Dimethylamine → HCID 86752155, 화합물

HRID 863701
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HRID 863701 반응식
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].C(O[CH2:20][CH:21]1[CH2:49][N:24]2[C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=3[C:31]([C:32]3[C:33](=O)[O:34][C:35](=[O:47])[C:36]=3[C:37]3[C:45]4[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=4)[N:39]([CH3:46])[CH:38]=3)=[C:23]2[CH2:22]1)(=O)C.[N:50]1C(C)=CC(C)=CC=1C.[CH3:59][NH:60][CH3:61]>ClCCl>[F:1][C:2]([F:15])([F:14])[S:3]([OH:6])(=[O:5])=[O:4].[CH3:59][N:60]([CH2:20][CH:21]1[CH2:49][N:24]2[C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=3[C:31]([C:32]3[C:33](=[O:34])[NH:50][C:35](=[O:47])[C:36]=3[C:37]3[C:45]4[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=4)[N:39]([CH3:46])[CH:38]=3)=[C:23]2[CH2:22]1)[CH3:61]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 674DimethylamineHCID 79532,4,6-TrimethylpyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 10004096HCID 10004096, 화합물

생성물 1

HCID 86752155HCID 86752155, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

546 mg of trifluoromethanesulphonic anhydride in 80 ml of dichloromethane were treated at 0° C. under a nitrogen atmosphere with a suspension of 400 mg of the product of Example 19 and 208 mg of collidine in 120 ml of dichloromethane. After 1 hour, 1.9 ml of 40% aqueous dimethylamine were added and the mixture was stirred for 3 hours. The solvent was removed and the residue was subjected to chromatography on silica gel with dichloromethane/methanol/acetone (88:10:2). Trituration with ethyl acetate followed by recrystallization from methanol gave 295 mg of 3-[2,3-dihydro-2-(dimethylaminomethyl)-1H-pyrrolo[1,2-a]indol-9-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione trifluoromethanesulphonate of melting point 323°-325° C.

후처리

  1. customThe solvent was removed
  2. customTrituration with ethyl acetate followed by recrystallization from methanol

출처 및 근거

ORD 기록
ord-beabd9295e7e47d1b875145e56da89a1
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05721245

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