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1,1'-Carbonyl-di-(1,2,4-triazole) → N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-6-((N-(2-(dimethylamino)ethyl)acetamido)methyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

HRID 1778001
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1778001
[NH2:1][C:2]1[CH:9]=[C:8]([NH:10][CH2:11][CH2:12][O:13][CH3:14])[C:5]([C:6]#[N:7])=[CH:4][N:3]=1.N1([C:20](N2C=NC=N2)=[O:21])C=NC=N1.[CH3:27][O:28][CH:29]([O:50][CH3:51])[C:30]1[C:39]([CH2:40][N:41]([CH2:45][CH2:46][N:47]([CH3:49])[CH3:48])[C:42](=[O:44])[CH3:43])=[CH:38][C:37]2[CH2:36][CH2:35][CH2:34][NH:33][C:32]=2[N:31]=1>CN(C=O)C>[C:6]([C:5]1[C:8]([NH:10][CH2:11][CH2:12][O:13][CH3:14])=[CH:9][C:2]([NH:1][C:20]([N:33]2[C:32]3[C:37](=[CH:38][C:39]([CH2:40][N:41]([CH2:45][CH2:46][N:47]([CH3:48])[CH3:49])[C:42](=[O:44])[CH3:43])=[C:30]([CH:29]([O:28][CH3:27])[O:50][CH3:51])[N:31]=3)[CH2:36][CH2:35][CH2:34]2)=[O:21])=[N:3][CH:4]=1)#[N:7]
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Komponenten

5

Edukt 3

HCID 43939611,1'-Carbonyl-di-(1,2,4-triazole)HCID 118036906N-((2-(dimethoxymethyl)-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)methyl)-N-(2-(dimethylamino)ethyl)acetamide2×HCID 1180369516-Amino-4-((2-methoxyethyl)amino)nicotinonitrile2×

Produkt 1

HCID 118036737N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-6-((N-(2-(dimethylamino)ethyl)acetamido)methyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 6-amino-4-((2-methoxyethyl)amino)nicotinonitrile (intermediate 75, 631 mg, 3.28 mmol) in anhydrous DMF (4 ml) was added drop wise to a mixture of di(1H-1,2,4-triazol-1-yl)methanone (539 mg, 3.28 mmol) and DMF (4 ml) cooled at 0° C. After stirring for 30 minutes at 0° C. the reaction mixture was allowed to warm to room temperature and stirred for approximately 2 h, after which a solution of N-((2-(dimethoxymethyl)-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)methyl)-N-(2-(dimethylamino)ethyl)acetamide (intermediate 198, 460 mg, 1.313 mmol) in DMF (4 ml) was added. The reaction mixture was continued to stir for 48 h at room temperature and quenched by pouring it into aqueous NaHCO3. The reaction mixture was diluted with EtOAc, phases were separated and the water phase was extracted with EtOAc and DCM. The combined organic phases were dried using Na2SO4, filtered and evaporated. The crude product was purified by reversed phase preparative HPLC eluting with a gradient of MeCN and water (RP 5, H2O/MeCN 70:30 to 40:60 in 25 min). Fractions containing the product were collected, diluted with water and basified with NaHCO3. The mixture was concentrated and extracted with DCM, dried using Na2SO4, filtered, concentrated and dried to yield the title compound as a colorless foamy solid. (UPLC-MS 3) tR 0.73 min, ESI-MS 569.0 [M+H]+. 1H NMR (600 MHz, DMSO-d6) (indicates an overlapping mixture of rotamers of the title compound in an approximate mixture of 0.6:0.4) δ 13.55 (s, 0.6H), 13.52 (s, 0.4H), 8.28 (s, 1H), 7.53 (s, 1H), 7.51 (s, 0.4H), 7.40 (s, 0.6H), 6.98-6.91 (m, 1H), 5.41 (s, 0.6H), 5.40 (s, 0.4H), 4.70 (s, 0.8H), 4.65 (s, 1.2H), 3.96-3.90 (m, 2H), 3.53 (t, 2H), 3.42-3.24 (m, 13H), 2.86 (t, 0.8H), 2.81 (t, 1.2H), 2.36 (t, 1.2H), 2.30 (t, 0.8H), 2.17-2.08 (m, 7.8H), 1.96 (s, 1.2H), 1.94-1.86 (m, 2H).

Aufarbeitung

  1. temperatureto warm to room temperature
  2. stirringstirred for approximately 2 h
  3. stirringto stir for 48 h at room temperature
  4. customquenched
  5. additionby pouring it into aqueous NaHCO3
  6. additionThe reaction mixture was diluted with EtOAc, phases
  7. customwere separated
  8. extractionthe water phase was extracted with EtOAc and DCM
  9. customThe combined organic phases were dried
  10. filtrationfiltered
  11. customevaporated
  12. customThe crude product was purified by reversed phase preparative HPLC
  13. washeluting with a gradient of MeCN and water (RP 5, H2O/MeCN 70:30 to 40:60 in 25 min)
  14. additionFractions containing the product
  15. customwere collected
  16. additiondiluted with water and basified with NaHCO3
  17. concentrationThe mixture was concentrated
  18. extractionextracted with DCM
  19. customdried
  20. filtrationfiltered
  21. concentrationconcentrated
  22. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a0ff8689e86d4bf6b7d88a9386b3c0bf
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09266883B2

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