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Water → 5-(2-Aminopyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

HRID 629102
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HRID 629102 반응식
Br[C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:21]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)=[O:8].CC1(C)C(C)(C)OB([C:30]2[CH:31]=[N:32][C:33]([NH2:36])=[N:34][CH:35]=2)O1.C([O-])([O-])=O.[K+].[K+].O>O1CCOCC1>[NH2:36][C:33]1[N:34]=[CH:35][C:30]([C:2]2[CH:3]=[N:4][CH:5]=[C:6]([CH:21]=2)[C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=2)=[O:8])=[CH:31][N:32]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 46840185-bromo-N-(4-(trifluoromethoxy)phenyl)nicotinamideHCID 177502122-Aminopyrimidine-5-boronic acid, pinacol ester

생성물 1

HCID 722035675-(2-Aminopyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

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온도
90 °C

실험 절차

5-Bromo-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 61.1, 181 mg, 0.5 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (133 mg, 0.6 mmol), PdCl2(dppf)-(CH2Cl2) (20.42 mg, 0.025 mmol), K2CO3 (138 mg, 1 mmol), water (2 mL) and dioxane (10 mL) were added to a vial, which was sealed, evacuated/purged with argon and the RM was stirred at 90° C. for 24 h. The solvent was evaporated off under reduced pressure and the residue was treated with water and extracted with EtOAc. The combined extracts were dried over Na2SO4 and the solvent was evaporated off under reduced pressure to give the product which was recrystallized from hot EtOAc to afford the title compound as a beige powder. UPLC-MS (Condition 2) tR 0.89 min, m/z=376.2 [M+H]+; 1H-NMR (400 MHz, DMSO-d6) δ ppm 6.98 (s, 2H) 7.41 (d, J=8.99 Hz, 2H) 7.90 (d, J=8.99 Hz, 2H) 8.50-8.55 (m, 1H) 8.76 (s, 2H) 9.00 (d, J=1.95 Hz, 1H) 9.06 (d, J=1.96 Hz, 1H) 10.62 (s, 1H).

후처리

  1. customwas sealed
  2. customevacuated/purged with argon
  3. customThe solvent was evaporated off under reduced pressure
  4. additionthe residue was treated with water
  5. extractionextracted with EtOAc
  6. dry with materialThe combined extracts were dried over Na2SO4
  7. customthe solvent was evaporated off under reduced pressure
  8. customto give the product which
  9. customwas recrystallized from hot EtOAc

출처 및 근거

ORD 기록
ord-b1b0b8e9abb0484c812bf8f6eb4b19a3
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315489B2

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