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Diisopropylethylamine → HCID 44541052, 화합물

HRID 1616025
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HRID 1616025 반응식
F[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])[CH:5]=[CH:4][CH:3]=1.[CH3:29][NH:30][CH:31]1[CH2:36][CH2:35][O:34][CH2:33][CH2:32]1.CCN(C(C)C)C(C)C>CS(C)=O.CO>[NH:24]1[C:25]2[C:21](=[C:20]([C:18]3[CH:17]=[C:16]4[C:12]([CH:13]=[N:14][NH:15]4)=[C:11]([NH:10][C:8]([C:6]4[CH:5]=[CH:4][CH:3]=[C:2]([N:30]([CH3:29])[CH:31]5[CH2:36][CH2:35][O:34][CH2:33][CH2:32]5)[N:7]=4)=[O:9])[CH:19]=3)[CH:28]=[CH:27][CH:26]=2)[CH:22]=[CH:23]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 69919504-(Methylamino)tetrahydro-2H-pyranHCID 44541051HCID 44541051, 화합물

생성물 1

HCID 44541052HCID 44541052, 화합물수율 26%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 887Methanol
용매

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온도
160 °C

실험 절차

6-Fluoro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-2-pyridinecarboxamide (50 mg, 0.14 mmol) and methyl(tetrahydro-2H-pyran-4-yl)amine (31 mg, 0.27 mmol) were dissolved in DMSO (0.5 ml) in a microwave vial. DIPEA (0.141 ml) was added and the mixture was heated at 160° C. for 4 h under microwave irradiation. The reaction mixture was diluted with MeOH (0.5 ml) and was purified by Mass Directed Automated Preparative HPLC (Method C). Fractions containing product were blown to dryness and the residue dissolved in methanol. This solution was loaded onto a 1 g aminopropyl column which was eluted with MeOH (1 column volume). The solvent was removed under a stream of nitrogen to give the title compound (17 mg) as a cream solid.

후처리

  1. customwas purified by Mass Directed Automated Preparative HPLC (Method C)
  2. additionFractions containing product
  3. dissolutionthe residue dissolved in methanol
  4. washwas eluted with MeOH (1 column volume)
  5. customThe solvent was removed under a stream of nitrogen

출처 및 근거

ORD 기록
ord-ab00c8b058eb48fdbce01806049dc81f
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765743B2

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