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Potassium Hydroxide → HCID 178464227、化合物

HRID 1014505
ノート
印刷プレビュー

反応式

HRID 1014505 の反応式
[CH2:1]([N:3]([CH3:50])[CH2:4][C:5]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([O:48][CH3:49])=[C:13]([NH:16][C:17]3[N:18]=[C:19]([NH:36][C:37]4[CH:46]=[CH:45][CH:44]=[C:43]([F:47])[C:38]=4[C:39]([NH:41][CH3:42])=[O:40])[C:20]4[CH:25]=[CH:24][N:23](S(C5C=CC(C)=CC=5)(=O)=O)[C:21]=4[N:22]=3)[CH:14]=2)[CH2:9][CH2:8]1)=[O:6])[CH3:2].[OH-].[K+]>O1CCOCC1.O>[CH2:1]([N:3]([CH3:50])[CH2:4][C:5]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([O:48][CH3:49])=[C:13]([NH:16][C:17]3[NH:22][C:21]4=[N:23][CH:24]=[CH:25][C:20]4=[C:19]([NH:36][C:37]4[CH:46]=[CH:45][CH:44]=[C:43]([F:47])[C:38]=4[C:39]([NH:41][CH3:42])=[O:40])[N:18]=3)[CH:14]=2)[CH2:9][CH2:8]1)=[O:6])[CH3:2]
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

5

反応物 2

HCID 14797Potassium HydroxideHCID 673168972-({2-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluoro-N-methylbenzamide

生成物 1

HCID 178464227HCID 178464227、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
92 °C

実験手順

5-Chloro-8-fluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one (0.6 g, 2.2 mmol) and 1-{[ethyl(methyl)amino]acetyl}-5-(methyloxy)-2,3-dihydro-1H-indol-6-amine (0.8 g, 1.8 mmol) were suspended in 50 ml of THF, the mixture was stirred at 82° C. overnight. The reaction mixture was cooled and diluted with 60 ml of ethyl acetate, and washed with saturated NaHCO3, the organic phase was dried over Na2SO4 and the solvent was removed to yield the 5-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-8-fluoro-3-[(4 methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one. The 5-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-8-fluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one was mixed with a solution of methylamine (2M in THF, 30 mL), the reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with 50 ml of ethyl acetate, and washed with saturated NaCl, the organic layer was dried over Na2SO4, and the solvents removed under reduced pressure to afford the corresponding 2-({2-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluoro-N-methylbenzamide. The 2-({2-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluoro-N-methylbenzamide was suspended in 15 ml of dioxane, then KOH was added (it was dissolved in 5 ml of water). The reaction mixture was stirred at 92° C. for 2 hours, the reaction mixture was cooled to room temperature, the solvent was removed, the residue was re-dissolved in 50 ml of CH2Cl2, and washed with water (2×100 ml). The combined organic phase was washed with a saturated NH4OH, then dried over Na2SO4, the solvent was removed to yield the crude product and purified by chromatography on SiO2 (0% to 10% MeOH/CH2Cl2 with 0.2% added NH3) to afford 2-[(2-{[1-(N-ethyl-N-methylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-1H-pyrrolo[2,3-d]pyrimidin-4-yl)amino]-6-fluoro-N-methylbenzamide as a yellow solid (0.26 g). 1H NMR (400 MHz), DMSO-d6) δ ppm 0.98 (t, J=6.59, 3H), 2.20 (s, 3H), 2.44 (t, J=7.33 Hz, 2H), 2.78 (d, J=3.11 Hz, 3H), 3.08 (t, J=7.51 Hz, 2H), 3.20 (s, 2H), 3.75 (s, 3H), 4.16 (t, J=7.79 Hz, 2H), 6.26 (s, 1H), 6.85-6.92 (m, 3H), 7.29 (q, J=7.05 Hz, 1H), 7.56 (s, 1H), 8.36 (d, J=8.15 Hz, 1H), 8.53 (s, 1H), 8.63 (s, 1H), 10.17 (s, 1H), 11.27 (s, 1H); ESIMS (M+H)+=547.

後処理

  1. temperaturethe reaction mixture was cooled to room temperature
  2. customthe solvent was removed
  3. dissolutionthe residue was re-dissolved in 50 ml of CH2Cl2
  4. washwashed with water (2×100 ml)
  5. washThe combined organic phase was washed with a saturated NH4OH
  6. dry with materialdried over Na2SO4
  7. customthe solvent was removed
  8. customto yield the crude product
  9. custompurified by chromatography on SiO2 (0% to 10% MeOH/CH2Cl2 with 0.2% added NH3)

出典と根拠

ORDレコード
ord-c92a0b4900574db886ecef47f319b91b
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981903B2

反応ノート

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