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Tetrabutylammonium Fluoride → HCID 89871088, 화합물

HRID 516175
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HRID 516175 반응식
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[C:19]([O:23][C:24]([N:26]([C:68]([O:70][C:71]([CH3:74])([CH3:73])[CH3:72])=[O:69])[C:27]1[C:28]2[C:35]([I:36])=[CH:34][N:33]([C@@H:37]3[CH2:41][N:40]([C:42]([O:44][C:45]([CH3:48])([CH3:47])[CH3:46])=[O:43])[C@H:39]([CH2:49][O:50][Si](C(C)(C)C)(C4C=CC=CC=4)C4C=CC=CC=4)[CH2:38]3)[C:29]=2[N:30]=[CH:31][N:32]=1)=[O:25])([CH3:22])([CH3:21])[CH3:20]>C1COCC1>[C:19]([O:23][C:24]([N:26]([C:68]([O:70][C:71]([CH3:74])([CH3:73])[CH3:72])=[O:69])[C:27]1[C:28]2[C:35]([I:36])=[CH:34][N:33]([C@@H:37]3[CH2:41][N:40]([C:42]([O:44][C:45]([CH3:46])([CH3:47])[CH3:48])=[O:43])[C@H:39]([CH2:49][OH:50])[CH2:38]3)[C:29]=2[N:30]=[CH:31][N:32]=1)=[O:25])([CH3:20])([CH3:21])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 89871072HCID 89871072, 화합물

생성물 1

HCID 89871088HCID 89871088, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Silica gel-carrying tetrabutyl ammonium fluoride (700 mg) (up to 1.5 mmol/g) was added to a solution of (2S,4S)-tert-butyl 4-(4-(bis(tert-butoxycarbonyl)amino)-5-iodo-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-2-((tert-butyldiphenylsilyloxy)methyl)pyrrolidine-1-carboxylate (237.5 mg) obtained in Step 3 in THF (5 ml), and the resulting mixture was stirred at room temperature overnight. Silica gel was separated by filtration, and the solvent of the filtrate was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate) to obtain the title compound as a light-yellow, amorphous substance (185 mg). Physical properties: m/z [M+H]+ 660.2

후처리

  1. customSilica gel was separated by filtration
  2. distillationthe solvent of the filtrate was distilled off under reduced pressure
  3. customThe resulting residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-bab0cd33d2494cf1895b1205d148c156
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09108973B2

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