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Ethanol → HCID 178515836, 화합물

HRID 1261991
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HRID 1261991 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][O:45][CH2:44][CH2:43]4)=[CH:38][CH:37]=3)=[N:33]2)=[CH:28][CH:27]=1.[OH:48][C:49]1[N:54]=[CH:53][C:52](B(O)O)=[CH:51][CH:50]=1.C(=O)([O-])[O-].[Na+].[Na+].O.C(O)C.[Cl-].[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[N:42]1([C:39]2[CH:40]=[CH:41][C:36]([NH:35][C:32]3[N:31]=[CH:30][C:29]4=[CH:28][CH:27]=[C:26]([C:52]5[CH:51]=[CH:50][C:49]([OH:48])=[N:54][CH:53]=5)[N:34]4[N:33]=3)=[CH:37][CH:38]=2)[CH2:47][CH2:46][O:45][CH2:44][CH2:43]1
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참가 물질

10

반응물 8

HCID 702EthanolHCID 962WaterHCID 5234Sodium ChlorideHCID 8028TetrahydrofuranHCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 54578326(7-Bromo-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-(4-morpholin-4-yl-phenyl)-amine
HCID 178514836
HCID 178514836, 화합물

생성물 1

HCID 178515836HCID 178515836, 화합물수율 5.2%

시약·촉매·용매 1

HCID 167845palladium(II) acetate촉매

실험 절차

Palladium Acetate (0.018 g, 0.000080 mol) and Triphenylphosphine (0.026 g, 0.00010 mol) were dissolved in Tetrahydrofuran (1.2 mL, 0.015 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-morpholin-4-yl-phenyl)-amine (0.150 g, 0.000401 mol) was then added and the reaction was again allowed to stir for 10 minutes. 6-hydroxy-3-pyridine boronic acid (0.111 g, 0.000802 mol) was added followed by 0.9 M of Sodium carbonate in water (1 mL, 0.0009 mol) and Ethanol (1.2 mL, 0.021 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 8.16 mg of 5-[2-(4-Morpholin-4-yl-phenylamino)-pyrrolo[2,1-f][1,2,4]triazin-7-yl]-pyridin-2-ol as a lyophilized powder. (M+H)=389.7. 1H NMR (400 MHz, DMSO, d6) δ 9.27 (s, 1H), 8.89 (s, 1H), 8.42 (m, 1H), 8.13 (dd, 1H, J=2.60, 7.00 Hz), 7.58 (d, 2H, J=8.92 Hz), 7.06 (m, 3H), 6.90 (d, 1H, J=4.76 Hz), 6.52 (d, 1H, J=9.61 Hz), 3.77 (m, 4H), 3.11 (m, 4H).

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-bb59a199742d4bd396386b41399cef7c
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08471005B2

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