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Water → HCID 66711984, 화합물

HRID 1262267
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HRID 1262267 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Br[C:21]1[N:29]2[C:24]([CH:25]=[N:26][C:27]([NH:30][C:31]3[CH:36]=[CH:35][C:34]([N:37]4[CH2:42][CH2:41][N:40]([CH3:43])[CH2:39][CH2:38]4)=[CH:33][CH:32]=3)=[N:28]2)=[CH:23][CH:22]=1.CC1(C)C(C)(C)OB([C:52]2[CH:61]=[CH:60][CH:59]=[CH:58][C:53]=2[O:54][CH2:55][C:56]#[N:57])O1.C(=O)([O-])[O-].[Na+].[Na+].O>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CN(C)C=O>[CH3:43][N:40]1[CH2:41][CH2:42][N:37]([C:34]2[CH:33]=[CH:32][C:31]([NH:30][C:27]3[N:26]=[CH:25][C:24]4=[CH:23][CH:22]=[C:21]([C:52]5[CH:61]=[CH:60][CH:59]=[CH:58][C:53]=5[O:54][CH2:55][C:56]#[N:57])[N:29]4[N:28]=3)=[CH:36][CH:35]=2)[CH2:38][CH2:39]1
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참가 물질

8

반응물 5

HCID 962WaterHCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 179989152-(2-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenoxy)acetonitrileHCID 66711200(7-Bromo-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine

생성물 1

HCID 66711984HCID 66711984, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6228Dimethylformamide용매

반응 조건

온도
55 °C

실험 절차

Into a 30 mL vial, Palladium Acetate (10 mg, 0.04 mmol), Triphenylphosphine (33 mg, 0.12 mmol) were added. The mixture was purged with nitrogen for 10 minutes. (7-Bromo-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-[4-(4-methyl-piperazin-1-yl)-phenyl]-amine (110.0 mg, 0.2840 mmol), [2-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenoxy]-acetonitrile (0.1472 g, 0.5681 mmol), N,N-Dimethylformamide (2.00 mL) and 1.50 M of Sodium carbonate in Water (2.0 mL, 3.0 mmol) were added. The reaction mixture was heated at 55° C. for 45 minutes. The reaction was partitioned with water and DCM. The organic was separated, washed with Brine and dried over Na2SO4. The solid was filtered and washed with DCM. The solvent was removed under vacuum. The desired product was isolated via ISCO column chromatography with DCM and methanol as eluant (0 to 15% methanol). The collected fractions afforded (2-{2-[4-(4-Methyl-piperazin-1-yl)-phenylamino]-pyrrolo[2,1-f][1,2,4]triazin-7-yl}-phenoxy)-acetonitrile as a yellow solid (65 mg, 52%). LCMS (E/I+) 440.2 (M+H). MP 95-101° C. NMR 1H (DMSO-d6)-9.16 (s, 1H), 8.92 (s, 1H), 7.88-7.98 (m, 1H), 7.48-7.58 (m, 3H), 7.34 (d, 1H, J=9.43), 7.26 (t, 1H, J=8.64 Hz), 6.94 (d, 1H, J=5.50), 6.90 (d, 1H, J=4.70 Hz), 6.81 (d, 2H, J=9.43 Hz), 5.19 (s, 2H), 3.03 (bs 3H), 2.45 (bs, 3H), 2.22 (s, 3H).

후처리

  1. customThe mixture was purged with nitrogen for 10 minutes
  2. customThe reaction was partitioned with water and DCM
  3. customThe organic was separated
  4. washwashed with Brine
  5. dry with materialdried over Na2SO4
  6. filtrationThe solid was filtered
  7. washwashed with DCM
  8. customThe solvent was removed under vacuum

출처 및 근거

ORD 기록
ord-7d282f8a64fc4cf992b570d56ebb8a12
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08471005B2

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