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Water → [7-(1,2-Dimethyl-1H-imidazol-4-yl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine

HRID 1262196
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HRID 1262196 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Br[C:21]1[N:22]=[C:23]([CH3:27])[N:24]([CH3:26])[CH:25]=1.[CH3:28][N:29]1[CH2:34][CH2:33][N:32]([C:35]2[CH:40]=[CH:39][C:38]([NH:41][C:42]3[N:47]=[CH:46][C:45]4=[CH:48][CH:49]=[C:50](B5OC(C)(C)C(C)(C)O5)[N:44]4[N:43]=3)=[CH:37][CH:36]=2)[CH2:31][CH2:30]1.C(=O)([O-])[O-].[Na+].[Na+].O>O1CCCC1.C(O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:26][N:24]1[CH:25]=[C:21]([C:50]2[N:44]3[C:45]([CH:46]=[N:47][C:42]([NH:41][C:38]4[CH:39]=[CH:40][C:35]([N:32]5[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]5)=[CH:36][CH:37]=4)=[N:43]3)=[CH:48][CH:49]=2)[N:22]=[C:23]1[CH3:27]
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참가 물질

9

반응물 5

HCID 962WaterHCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 72048754-Bromo-1,2-dimethyl-1H-imidazoleHCID 57416042N-[4-(4-methylpiperazin-1-yl)phenyl]-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrrolo[2,1-f][1,2,4]triazin-2-amine

생성물 1

HCID 66712164
[7-(1,2-Dimethyl-1H-imidazol-4-yl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine
수율 23%

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Palladium acetate (13.0 mg, 0.0580 mmol) and triphenylphosphine (19.0 mg, 0.0725 mmol) were placed in tetrahydrofuran (2.00 mL). The mixture was allowed to stir at room temperature for 10 minutes. 4-Bromo-1,2-dimethyl-1H-imidazole (102 mg, 0.580) was then added and the reaction was again allowed to stir for 10 minutes. [4-(4-Methyl-piperazin-1-yl)-phenyl]-[7-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-amine (105 mg, 0.242 mmol) was added followed by 1.50 M sodium carbonate in water (0.645 mL, 0.967 mmol) and ethanol (2.00 mL). The reaction mixture was then heated at 80° C. overnight. The reaction was partitioned between DCM (50 mL) and water (50 mL). The organic layer was washed twice with water (50 mL) and then dried over sodium sulfate, filtered, and concentrated under reduced pressure. Purification by prep-HPLC using a gradient of 10-45% AcN/water both containing 0.1% TFA as the eluting solvent. The product was then free based to obtain the title compound as a yellow solid (22 mg, 23%). m.p.=242-244° C.; LCMS (m/e) 403 (M+H); 1H-NMR (CDCl3, 400 MHz) δ 8.61 (s, 1H), 7.84 (s, 1H), 7.57-7.50 (m, 2H), 7.24 (d, 1H, J=4.8 Hz), 7.02-6.95 (m, 2H), 6.80 (d, 1H, J=4.8 Hz), 6.55 (bs, 1H), 3.62 (s, 3H), 3.24-3.16 (m, 4H), 2.65-2.57 (m, 4H), 2.46 (s, 3H), 2.38 (s, 3H).

후처리

  1. stirringto stir for 10 minutes
  2. temperatureThe reaction mixture was then heated at 80° C. overnight
  3. customThe reaction was partitioned between DCM (50 mL) and water (50 mL)
  4. washThe organic layer was washed twice with water (50 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customPurification

출처 및 근거

ORD 기록
ord-95caf10fa33542c784c05d32a02903c9
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08471005B2

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