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Diisopropylethylamine → HCID 44541052、化合物

HRID 1616025
ノート
印刷プレビュー

反応式

HRID 1616025 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 69919504-(Methylamino)tetrahydro-2H-pyranHCID 44541051HCID 44541051、化合物

生成物 1

HCID 44541052HCID 44541052、化合物収率 26%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 887Methanol
溶媒

反応条件

温度
160 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ab00c8b058eb48fdbce01806049dc81f
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765743B2

反応ノート

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