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Ethanol → N-Methyl-3-{2-[4-(4-methyl-piperazin-1-yl)-phenylamino]-pyrrolo[2,1-f][1,2,4]triazin-7-yl}-benzenesulfonamide

HRID 1262015
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HRID 1262015 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O1CCCC1.Br[C:26]1[N:34]2[C:29]([CH:30]=[N:31][C:32]([NH:35][C:36]3[CH:41]=[CH:40][C:39]([N:42]4[CH2:47][CH2:46][N:45]([CH3:48])[CH2:44][CH2:43]4)=[CH:38][CH:37]=3)=[N:33]2)=[CH:28][CH:27]=1.[CH3:49][NH:50][S:51]([C:54]1[CH:59]=[CH:58][CH:57]=[C:56](B(O)O)[CH:55]=1)(=[O:53])=[O:52].C(=O)([O-])[O-].[Na+].[Na+].O.C(O)C.[Cl-].[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:49][NH:50][S:51]([C:54]1[CH:55]=[CH:56][CH:57]=[C:58]([C:26]2[N:34]3[C:29]([CH:30]=[N:31][C:32]([NH:35][C:36]4[CH:37]=[CH:38][C:39]([N:42]5[CH2:43][CH2:44][N:45]([CH3:48])[CH2:46][CH2:47]5)=[CH:40][CH:41]=4)=[N:33]3)=[CH:28][CH:27]=2)[CH:59]=1)(=[O:52])=[O:53]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 8

HCID 702EthanolHCID 962WaterHCID 5234Sodium ChlorideHCID 8028TetrahydrofuranHCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 44886921Methyl 3-boronobenzenesulfonamide
HCID 66711200
(7-Bromo-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine

생성물 1

HCID 66711491N-Methyl-3-{2-[4-(4-methyl-piperazin-1-yl)-phenylamino]-pyrrolo[2,1-f][1,2,4]triazin-7-yl}-benzenesulfonamide수율 24.7%

시약·촉매·용매 1

HCID 167845palladium(II) acetate촉매

실험 절차

Palladium Acetate (0.017 g, 0.000077 mol) and Triphenylphosphine (0.025 g, 0.000097 mol) were dissolved in Tetrahydrofuran (1.2 mL, 0.014 mol) and the mixture was allowed to stir at room temperature for 10 minutes. (7-Bromo-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine (0.125 g, 0.000323 mol) was then added and the reaction was again allowed to stir for 10 minutes. N-methyl-3-boronobenzenesulfonamide (0.166 g, 0.000775 mol) was added followed by 0.9 M of Sodium carbonate in water (0.9 mL, 0.0008 mol) and Ethanol (1.2 mL, 0.020 mol). The reaction mixture was then heated at 80° C. and was allowed to stir overnight. The reaction mixture was poured over saturated sodium chloride, and organics were extracted with ethyl acetate. Combined organics were dried over sodium sulfate, filtered and reduced en vacuo. The crude mixture was purified by Gilson prep HPLC to afford 38.12 mg of N-Methyl-3-{2-[4-(4-methyl-piperazin-1-yl)-phenylamino]-pyrrolo[2,1-f][1,2,4]triazin-7-yl}-benzenesulfonamide as a lyophilized powder. (M+H)=478.1. 1H NMR (400 MHz, DMSO, d6) δ 9.74 (s, 1H), 9.40 (s, 1H), 9.02 (s, 1H), 8.53 (s, 1H), 8.40 (m, 1H), 7.76 (m, 2H), 7.68 (m, 2H), 7.55 (m, 1H), 7.19 (d, 1H, J=4.28 Hz), 7.04 (m, 1H), 6.98 (d, 1H, J=4.32 Hz), 3.72 (m, 2H), 3.53 (m, 2H), 3.20 (m, 2H), 2.94 (m, 2H), 2.91 (s, 3H), 2.40 (s, 3H).

후처리

  1. stirringto stir for 10 minutes
  2. temperatureThe reaction mixture was then heated at 80° C.
  3. stirringto stir overnight
  4. extractionorganics were extracted with ethyl acetate
  5. dry with materialCombined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. customThe crude mixture was purified by Gilson prep HPLC

출처 및 근거

ORD 기록
ord-efbe047913b54e91bcac7f5f7750704a
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08471005B2

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