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Methylamine → 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

HRID 1014504
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HRID 1014504 반응식
[CH2:1]([N:3]([CH3:48])[CH2:4][C:5]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([O:46][CH3:47])=[C:13]([NH:16][C:17]3[N:30]4[C:21](=[N:22][C:23]5[C:28]([C:29]4=[O:31])=[C:27]([F:32])[CH:26]=[CH:25][CH:24]=5)[C:20]4[CH:33]=[CH:34][N:35]([S:36]([C:39]5[CH:44]=[CH:43][C:42]([CH3:45])=[CH:41][CH:40]=5)(=[O:38])=[O:37])[C:19]=4[N:18]=3)[CH:14]=2)[CH2:9][CH2:8]1)=[O:6])[CH3:2].[CH3:49][NH2:50]>C(OCC)(=O)C>[CH2:1]([N:3]([CH3:48])[CH2:4][C:5]([N:7]1[C:15]2[C:10](=[CH:11][C:12]([O:46][CH3:47])=[C:13]([NH:16][C:17]3[N:30]=[C:21]([NH:22][C:23]4[CH:24]=[CH:25][CH:26]=[C:27]([F:32])[C:28]=4[C:29]([NH:50][CH3:49])=[O:31])[C:20]4[CH:33]=[CH:34][N:35]([S:36]([C:39]5[CH:44]=[CH:43][C:42]([CH3:45])=[CH:41][CH:40]=5)(=[O:37])=[O:38])[C:19]=4[N:18]=3)[CH:14]=2)[CH2:9][CH2:8]1)=[O:6])[CH3:2]
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 673167115-{[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

생성물 1

HCID 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

시약·촉매·용매 1

HCID 8857
Ethyl Acetate
용매

실험 절차

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.

후처리

  1. washwashed with saturated NaCl
  2. dry with materialthe organic layer was dried over Na2SO4
  3. customthe solvents removed under reduced pressure

출처 및 근거

ORD 기록
ord-363bd1470f944fd3ad9ef8b6763afade
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981903B2

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