Piperidine → HCID 44539729, 화합물

HRID 1616032노트

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HRID 1616032 반응식
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:10][C:11]2[CH:19]=[C:18]([C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[CH:17]=[C:16]3[C:12]=2[CH:13]=[N:14][NH:15]3)=[O:9])[C:5](F)=[CH:4][CH:3]=1.[NH:30]1[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1.CCN(C(C)C)C(C)C>CS(C)=O.CS(C)=O.CO>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:10][C:11]2[CH:19]=[C:18]([C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[CH:17]=[C:16]3[C:12]=2[CH:13]=[N:14][NH:15]3)=[O:9])[C:5]([N:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 8082PiperidineHCID 81531DiisopropylethylamineHCID 44540868HCID 44540868, 화합물

생성물 1

HCID 44539729HCID 44539729, 화합물수율 13.6%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 22036561Dimethyl sulfoxide methanol용매

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온도
160 °C

실험 절차

To a microwave vial was added 2 ml of a solution of 6-chloro-3-fluoro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-2-pyridinecarboxamide (300 mg, 0.74 mmol) in DMSO (6 ml). Piperidine (0.024 ml, 0.25 mmol) and DIPEA (0.129 ml) were added and the mixture was heated at 160° C. for 2 h under microwave irradiation. The crude reaction mixture was dissolved in DMSO/MeOH (1:1) and purified by Mass Directed Automated Preparative HPLC (Method E). The sample was further purified by Mass Directed Automated Preparative HPLC (Method E) and product-containing fractions were dried under a stream of nitrogen to afford the title compound (16 mg).

후처리

  1. customThe crude reaction mixture
  2. custompurified by Mass Directed Automated Preparative HPLC (Method E)
  3. customThe sample was further purified by Mass Directed Automated Preparative HPLC (Method E)
  4. additionproduct-containing fractions
  5. customwere dried under a stream of nitrogen

출처 및 근거

ORD 기록
ord-fe02c776bf7a40108f84c0d0980b7eed
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765743B2

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