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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
ノート
印刷プレビュー

反応式

HRID 419676 の反応式
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]
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

7

反応物 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

生成物 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
収率 48.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 64092,2,2-Trifluoroethanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-12d7eed28c1441e8aa083102da6b50e7
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093239B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート