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Hydrochloric Acid → HCID 59441879, 화합물

HRID 1014463
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HRID 1014463 반응식
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:14][CH3:15])=[C:10]([NH2:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].Cl[C:17]1[N:18]=[C:19]([NH:36][C:37]2[CH:45]=[CH:44][CH:43]=[C:42]([F:46])[C:38]=2[C:39]([NH2:41])=[O:40])[C:20]2[CH:25]=[CH:24][N:23]([S:26]([C:29]3[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][CH:30]=3)(=[O:28])=[O:27])[C:21]=2[N:22]=1.Cl.O1CCOCC1.[NH4+].[OH-]>FC(F)(F)CO.C1COCC1>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:14][CH3:15])=[C:10]([NH:13][C:17]3[N:18]=[C:19]([NH:36][C:37]4[CH:45]=[CH:44][CH:43]=[C:42]([F:46])[C:38]=4[C:39]([NH2:41])=[O:40])[C:20]4[CH:25]=[CH:24][N:23]([S:26]([C:29]5[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][CH:30]=5)(=[O:27])=[O:28])[C:21]=4[N:22]=3)[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
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참가 물질

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반응물 5

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 312751,4-DioxaneHCID 594418241-(6-Amino-5-methoxyindolin-1-yl)ethanoneHCID 866441882-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzamide

생성물 1

HCID 59441879HCID 59441879, 화합물

시약·촉매·용매 2

HCID 64092,2,2-Trifluoroethanol용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

A slurry of 1-acetyl-5-(methyloxy)-2,3-dihydro-1H-indol-6-amine (212 mg, 2 mmol), 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzamide (836 mg, 1.8 mmol), KI (5.6 mg, 0.03 mmol) in 2,2,2-trifluoroethanol (10 mL) was treated with a 4 N HCl solution in dioxane (1.8 mL, 7.2 mmol). The reaction mixture was heated at 80° C. overnight in a sealed vessel, then was allowed to cool to rt Half of the reaction mixture was diluted with THF (100 mL) and a 27% aqueous NH4OH solution (100 mL). After stirring at rt overnight the reaction mixture was concentrated to dryness. The residue was sonicated in CH2Cl2 (10 mL), then filtered. The filtrate was purified by silica gel chromatography using 8-10% THF/CH2Cl2 to obtain 2-({2-{[1-acetyl-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzamide as a yellow solid (192 mg, 34% for 2 steps). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.16 (s, 3H), 2.35 (s, 3H), 3.19 (t, J=8.33 Hz, 2H), 3.73 (s, 3H), 4.15 (t, J=8.33 Hz, 2H), 6.50 (d, J=3.85 Hz, 1H), 6.92 (t, J=9.25 Hz, 1H), 7.04 (s, 1H), 7.15-7.40 (m, 4H), 7.90-7.99 (m, 3H), 8.02 (s, 1H), 8.10 (d, J=8.61 Hz, 1H), 8.16 (s, 1H), 8.24 (s, 1H), 10.49 (s, 1H); ESIMS (M+H)+=630.13.

후처리

  1. temperatureto cool to rt Half of the reaction mixture
  2. concentrationwas concentrated to dryness
  3. customThe residue was sonicated in CH2Cl2 (10 mL)
  4. filtrationfiltered
  5. customThe filtrate was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-a064ee7c9c004004844c2d35aaa8808c
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981903B2

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