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1-Fluoro-2,6-dichloropyridinium Triflate → HCID 67155968, 화합물

HRID 2196717
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HRID 2196717 반응식
[O-]S(C(F)(F)[F:6])(=O)=O.F[N+]1C(Cl)=CC=CC=1Cl.[F:18][C:19]1[C:36]([NH:37][S:38]([CH2:41][CH2:42][CH3:43])(=[O:40])=[O:39])=[CH:35][CH:34]=[C:33]([F:44])[C:20]=1[C:21]([NH:23][C:24]1[CH:25]=[C:26]2[CH:32]=[CH:31][NH:30][C:27]2=[N:28][CH:29]=1)=[O:22]>CC#N.CCOC(C)=O>[F:18][C:19]1[C:36]([NH:37][S:38]([CH2:41][CH2:42][CH3:43])(=[O:40])=[O:39])=[CH:35][CH:34]=[C:33]([F:44])[C:20]=1[C:21]([NH:23][C:24]1[CH:25]=[C:26]2[C:32]([F:6])=[CH:31][NH:30][C:27]2=[N:28][CH:29]=1)=[O:22]
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참가 물질

5

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HCID 27373111-Fluoro-2,6-dichloropyridinium TriflateHCID 441994082,6-difluoro-3-(propylsulfonamido)-N-(1H-pyrrolo[2,3-b]pyridin-5-yl)benzamide

생성물 1

HCID 67155968HCID 67155968, 화합물수율 26%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

1-Fluoro-2,6-dichloropyridinium triflate (31 mg, 0.1 mmol) was added to 2,6-difluoro-N-(1H-pyrrolo[2,3-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (39 mg, 0.1 mmol) in MeCN (4 mL). The mixture was heated at 60° C. for 18 hours and then cooled to room temperature. The mixture was then diluted with EtOAc, washed with brine, dried over MgSO4 and concentrated. The crude product was purified using silica gel chromatography (ISCO) using 5% MeOH in CH2Cl2 as eluent, and subsequently reverse phase HPLC to give 2,6-difluoro-N-(3-fluoro-1H-pyrrolo[2,3-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (10.7 mg, 26%). 1H NMR (400 MHz, d6-DMSO) δ 11.51 (s, 3H), 10.97 (s, 3H), 9.77 (s, 3H), 8.41 (s, 6H), 7.70-7.38 (m, 6H), 7.26 (t, J=8.5, 3H), 3.45-2.96 (m, 32H), 2.50 (s, 57H), 2.36-2.09 (m, 1H), 1.77 (dd, J=7.5, 15.1, 6H), 1.00 (t, J=7.4, 9H); m/z (LC-MS) M+1=413.4.

후처리

  1. temperaturecooled to room temperature
  2. washwashed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe crude product was purified

출처 및 근거

ORD 기록
ord-bee7837bd4484fb0a10218be4f50b4f3
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338452B2

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