Diisopropylethylamine → HCID 44539634, 화합물

HRID 1616026노트

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HRID 1616026 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][N:30]1[CH2:35][CH2:34][CH:33]([NH2:36])[CH2:32][CH2:31]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]([NH:36][CH:33]5[CH2:34][CH2:35][N:30]([CH3:29])[CH2:31][CH2:32]5)[N:7]=4)=[O:9])[CH:19]=3)[CH:28]=[CH:27][CH:26]=2)[CH:22]=[CH:23]1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 27375314-Amino-1-methylpiperidineHCID 44541051HCID 44541051, 화합물

생성물 1

HCID 44539634HCID 44539634, 화합물수율 43%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 887Methanol용매

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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 1-methyl-4-piperidinamine (30.7 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 removed under a stream of nitrogen to give the title compound (28 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 removed under a stream of nitrogen

출처 및 근거

ORD 기록
ord-368afee83f7b45ab87ee2c6ef09b81d4
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765743B2

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