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3-Aminopyridine → HCID 89650076, 화합물

HRID 2174240
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HRID 2174240 반응식
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[C:4]([NH:13][C:14]([NH:16][CH2:17][CH3:18])=[O:15])[CH:3]=1.[NH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.CC([O-])=O.CC([O-])=O.[Pd+2].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[CH2:17]([NH:16][C:14](=[O:15])[NH:13][C:4]1[CH:3]=[C:2]([NH:19][C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=1)[CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 100093-AminopyridineHCID 10796Cesium carbonateHCID 89651155HCID 89651155, 화합물

생성물 1

HCID 89650076HCID 89650076, 화합물수율 66%

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매
HCID 636044
1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)
촉매
HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

To a solution of ethyl 4-chloro-6-(3-ethylureido)nicotinate, i (1.0 g, 3.70 mmol), in 1,4-dioxane (25 mL) was added 3-aminopyridine (0.435 g, 4.81 mmol) followed by Cs2CO3 (1.80 g, 5.55 mmol). The resulting solution was purged with nitrogen for 15 min followed by addition of Pd(OAc)2 (0.025 g, 0.11 mmol) and Xantphos (0.13 g, 0.22 mmol). The reaction mixture was again purged with nitrogen for 15 min and then heated at 80° C. overnight. The reaction mixture was cooled to room temperature, filtered through a celite bed, and the bed washed with EtOAc. The combined filtrate was concentrated under reduced pressure. Water was added to the residue and the mixture extracted with EtOAc (3×50 mL). The combined organic phase was washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The crude product thus obtained was triturated with a mixture of 10% MeOH-Et2O to obtain compound ii as an off-white solid (0.80 g, 66%). 1H NMR (DMSO-d6, 400 MHz): δ 9.62 (s, 1H), 9.17 (s, 1H), 8.63 (s, 1H), 8.56 (d, J=2.4 Hz, 1H), 8.41 (d, J=4.4 Hz, 1H), 7.77 (m, 1H), 7.75 (br s, 1H), 7.48 (m, 1H), 7.20 (s, 1H), 4.32 (q, J=6.8 Hz, 2H), 3.11 (q, J=7.20 Hz, 2H), 1.33 (t, J=6.8 Hz, 3H) and 1.03 (t, J=7.20 Hz, 3H). [M+H]+ m/z=330.12.

후처리

  1. customThe resulting solution was purged with nitrogen for 15 min
  2. customThe reaction mixture was again purged with nitrogen for 15 min
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationfiltered through a celite bed
  5. washthe bed washed with EtOAc
  6. concentrationThe combined filtrate was concentrated under reduced pressure
  7. additionWater was added to the residue
  8. extractionthe mixture extracted with EtOAc (3×50 mL)
  9. washThe combined organic phase was washed with brine
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. customThe crude product thus obtained
  14. customwas triturated with a mixture of 10% MeOH-Et2O

출처 및 근거

ORD 기록
ord-7e5100a2c283412cae8e4367d10ec246
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09060515B2

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