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Ammonia → N-(2,6-difluorophenyl)-5-[3-(2-{[4-{(3S)-3-(1-methylethyl)-4-[2-(methylsulfonyl)-ethyl]-1-piperazinyl}-2-(methyloxy)phenyl]amino}-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-2-(methyloxy)benzamide

HRID 419676
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HRID 419676 반응식
Cl[C:2]1[N:7]=[C:6]([C:8]2[N:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]3=[N:10][C:9]=2[C:17]2[CH:18]=[CH:19][C:20]([O:34][CH3:35])=[C:21]([CH:33]=2)[C:22]([NH:24][C:25]2[C:30]([F:31])=[CH:29][CH:28]=[CH:27][C:26]=2[F:32])=[O:23])[CH:5]=[CH:4][N:3]=1.[CH3:36][CH:37]([C@@H:39]1[N:44]([CH2:45][CH2:46][S:47]([CH3:50])(=[O:49])=[O:48])[CH2:43][CH2:42][N:41]([C:51]2[CH:57]=[CH:56][C:54]([NH2:55])=[C:53]([O:58][CH3:59])[CH:52]=2)[CH2:40]1)[CH3:38].Cl.N>C(O)C(F)(F)F.CO>[F:32][C:26]1[CH:27]=[CH:28][CH:29]=[C:30]([F:31])[C:25]=1[NH:24][C:22](=[O:23])[C:21]1[CH:33]=[C:17]([C:9]2[N:10]=[C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][N:12]3[C:8]=2[C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH:55][C:54]3[CH:56]=[CH:57][C:51]([N:41]4[CH2:42][CH2:43][N:44]([CH2:45][CH2:46][S:47]([CH3:50])(=[O:49])=[O:48])[C@@H:39]([CH:37]([CH3:38])[CH3:36])[CH2:40]4)=[CH:52][C:53]=3[O:58][CH3:59])[N:7]=2)[CH:18]=[CH:19][C:20]=1[O:34][CH3:35]
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 594525905-(3-(2-chloropyrimidin-4-yl)imidazo[1,2-a]pyridin-2-yl)-N-(2,6-difluorophenyl)-2-methoxybenzamideHCID 666500244-{(3S)-3-(1-methylethyl)-4-[2-(methylsulfonyl)ethyl)-1-piperazinyl]-2-(methyloxy)aniline

생성물 1

HCID 59452920
N-(2,6-difluorophenyl)-5-[3-(2-{[4-{(3S)-3-(1-methylethyl)-4-[2-(methylsulfonyl)-ethyl]-1-piperazinyl}-2-(methyloxy)phenyl]amino}-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-2-(methyloxy)benzamide
수율 48.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 64092,2,2-Trifluoroethanol용매

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온도
80 °C

실험 절차

To 5-[3-(2-Chloro-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-N-(2,6-difluorophenyl)-2-(methyloxy)benzamide (Intermediate Example 2) (0.241 g, 0.490 mmol) and 4-{(3S)-3-(1-methylethyl)-4-[2-(methylsulfonyl)ethyl]-1-piperazinyl}-2-(methyloxy)aniline (0.174 g, 0.489 mmol) were dissolved in 5 mL of trifluoroethanol with stirring in a pressure vessel. Hydrogen chloride (0.49 mL, 4N in dioxane, 2.0 mmol) was added, and the vessel was sealed. The reaction was heated to 80° C. for 3 days and subsequently cooled to rt. The reaction was poured into 10 mL of 7N NH3 in MeOH and concentrated onto silica gel. The compound was purified by flash chromatography, and the fractions containing the desired compound were concentrated in vacuo. The material was triturated with diethyl ether, filtered, and washed with diethyl ether. The solid was collected to afford the title compound (0.191 g, 0.236 mmol, 48%). 1H NMR (400 MHz, DMSO-d6) δ ppm 9.75 (s, 1H), 9.33 (br. s., 1H), 8.42 (s, 1H), 8.17 (d, J=5.1 Hz, 1H), 8.03-8.09 (m, 1H), 7.70-7.78 (m, 1H), 7.66 (d, J=9.0 Hz, 1H), 7.29-7.43 (m, 3H), 7.25 (d, J=8.8 Hz, 1H), 7.10-7.19 (m, 2H), 6.87-6.95 (m, 1H), 6.61 (s, 1H), 6.43-6.52 (m, 2H), 3.95 (s, 3H), 3.77 (s, 3H), 3.43-3.51 (m, 1H), 3.30-3.41 (m, 2H), 3.27 (s, 3H), 2.99 (s, 3H), 2.91-2.98 (m, 1H), 2.68-2.85 (m, 2H), 2.51-2.60 (m, 1H), 2.22-2.30 (m, 1H), 2.05-2.16 (m, 1H), 0.96 (d, J=6.8 Hz, 3H), 0.87 (d, J=7.0 Hz, 3H). MS (M+H, ES+) 811.

후처리

  1. customthe vessel was sealed
  2. temperaturesubsequently cooled to rt
  3. concentrationconcentrated onto silica gel
  4. customThe compound was purified by flash chromatography
  5. additionthe fractions containing the desired compound
  6. concentrationwere concentrated in vacuo
  7. customThe material was triturated with diethyl ether
  8. filtrationfiltered
  9. washwashed with diethyl ether
  10. customThe solid was collected

출처 및 근거

ORD 기록
ord-12d7eed28c1441e8aa083102da6b50e7
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093239B2

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