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3-Aminopyridine → HCID 89650076、化合物

HRID 2174240
ノート
印刷プレビュー

反応式

HRID 2174240 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 100093-AminopyridineHCID 10796Cesium carbonateHCID 89651155HCID 89651155、化合物

生成物 1

HCID 89650076HCID 89650076、化合物収率 66%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 636044
1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7e5100a2c283412cae8e4367d10ec246
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09060515B2

反応ノート

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