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Water → N-(4-fluorophenyl)-N'-[3-fluoro-4-(7H-pyrrolo[2,3-d]pyrimidin-4-yloxy)phenyl]propanediamide

HRID 1011289
ノート
印刷プレビュー

反応式

HRID 1011289 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH2:18])[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[C:10]2[CH:17]=[CH:16][NH:15][C:11]=2[N:12]=[CH:13][N:14]=1.CN(C(ON1N=N[C:29]2[CH:30]=[CH:31][CH:32]=N[C:28]1=2)=[N+](C)C)C.[F:36][P-](F)(F)(F)(F)F.C(N([CH2:48][CH3:49])CC)C.[CH3:50][N:51]([CH:53]=[O:54])C.[OH2:55]>>[F:36][C:30]1[CH:31]=[CH:32][C:50]([NH:51][C:53](=[O:54])[CH2:48][C:49]([NH:18][C:4]2[CH:5]=[CH:6][C:7]([O:8][C:9]3[C:10]4[CH:17]=[CH:16][NH:15][C:11]=4[N:12]=[CH:13][N:14]=3)=[C:2]([F:1])[CH:3]=2)=[O:55])=[CH:28][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 589380223-fluoro-4-(7H-pyrrolo[2,3-d]pyrimidin-4-yloxy)-phenylamine

生成物 1

HCID 11568014
N-(4-fluorophenyl)-N'-[3-fluoro-4-(7H-pyrrolo[2,3-d]pyrimidin-4-yloxy)phenyl]propanediamide
収率 21%

実験手順

To a round bottom flask equipped with a magnetic stir bar was added 3-fluoro-4-(7H-pyrrolo[2,3-d]pyrimidin-4-yloxy)-phenylamine (0.141 mg, 0.57 mmol, 1.0 eq.), 1-(4-fluoro-phenylcarbamoyl)-carboxylic acid (0.193 g, 0.88 mmol), HATU (0.584 g, 1.14 mmol), triethylamine (0.23 ml, 1.3 mmol) and anhydrous DMF (5 ml). The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with H2O (100 ml) and extracted with CHCl3 (3×). The combined organic extractions were washed with H2O (1×), sat'd NaHCO3 (2×), 10% LiCl (3×), sat'd NaCl (1×), dried (Na2SO4), and concentrated in vacuo. The resulting crude residue was purified by HPLC to yield N-(4-fluorophenyl)-N′-[3-fluoro-4-(7H-pyrrolo[2,3-d]pyrimidin-4-yloxy)phenyl]propanediamide as a white solid (0.051 g, 21% yield). 1H NMR (400 MHz, DMSO): 12.30 (s, 1H), 10.49 (s, 1H), 10.28 (s, 1H), 8.29(s, 1H), 7.80 (dd, 1H), 7.65 (m, 2H), 7.51 (m, 1H), 7.40 (m, 2H), 7.19 (m, 2H), 6.58 (d, 1H), 3.49 (s, 2H); MS (ESI) for C21H15F2N5O3: 424 (MH+).

後処理

  1. customTo a round bottom flask equipped with a magnetic stir bar
  2. extractionextracted with CHCl3 (3×)
  3. extractionThe combined organic extractions
  4. washwere washed with H2O (1×), sat'd NaHCO3 (2×), 10% LiCl (3×), sat'd NaCl (1×)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customThe resulting crude residue was purified by HPLC

出典と根拠

ORDレコード
ord-e843c13aa865475c886b3bcfbf0dead6
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977345B2

反応ノート

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