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Trifluoromethanesulfonic acid → 1-(5-(3-(4-Amino-6-methyl-1,3,5-triazin-2-yl)pyridin-2-ylamino)pyridin-2-yl)-3-isopropylurea

HRID 1812092
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1812092
COC1C=CC(C[N:8](CC2C=CC(OC)=CC=2)[C:9]2[N:14]=[C:13]([CH3:15])[N:12]=[C:11]([C:16]3[C:17]([NH:22][C:23]4[CH:24]=[CH:25][C:26]([NH:29][C:30]([NH:32][CH:33]([CH3:35])[CH3:34])=[O:31])=[N:27][CH:28]=4)=[N:18][CH:19]=[CH:20][CH:21]=3)[N:10]=2)=CC=1.FC(F)(F)S(O)(=O)=O>C(O)(C(F)(F)F)=O>[NH2:8][C:9]1[N:14]=[C:13]([CH3:15])[N:12]=[C:11]([C:16]2[C:17]([NH:22][C:23]3[CH:24]=[CH:25][C:26]([NH:29][C:30]([NH:32][CH:33]([CH3:35])[CH3:34])=[O:31])=[N:27][CH:28]=3)=[N:18][CH:19]=[CH:20][CH:21]=2)[N:10]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 62406Trifluoromethanesulfonic acid2×HCID 666003931-(5-(3-(4-(Bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)pyridin-2-ylamino)pyridin-2-yl)-3-isopropylurea

Produkt 1

HCID 595482531-(5-(3-(4-Amino-6-methyl-1,3,5-triazin-2-yl)pyridin-2-ylamino)pyridin-2-yl)-3-isopropylureaAusbeute 49 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acid
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A stirred solution of 1-(5-(3-(4-(bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)pyridin-2-ylamino)pyridin-2-yl)-3-isopropylurea (0.104 g, 0.168 mmol) in TFA (2 mL) was treated with trifluoromethanesulfonic acid (TCI) (0.02 mL, 0.2 mmol) and the reaction mixture was stirred at 70° C. for 2 h, then 80° C. for 2 h. TFA (2 mL) and trifluoromethanesulfonic acid (0.05 mL) were added. The heating was resumed at 75° C. for another 2 h. The mixture was cooled to rt, and some of the TFA was removed in vacuo. Sat'd NaHCO3 was added slowly until effervescence was no longer observed. The aqueous phase was extracted with 25% iPrOH in CHCl3+1% NH4OH (3×10 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by silica gel chromatography (25 g, eluent: iPrOH (w/10% NH4OH) in CHCl3 0%-10%) to give 1-(5-(3-(4-amino-6-methyl-1,3,5-triazin-2-yl)pyridin-2-ylamino)pyridin-2-yl)-3-isopropylurea (0.0312 g, 49% yield) as a yellow powder. 1H NMR (300 MHz, d6-DMSO) δ 11.77 (s, 1H); 8.92 (s, 1H); 8.77 (d, J=7.75 Hz, 1H); 8.65 (br. s., 1H); 8.31 (br. s., 1H); 8.10 (br. s., 1H); 7.85 (br. s., 2H); 7.71 (br. s., 1H); 7.38 (d, J=8.92 Hz, 1H); 6.80-6.99 (m, 1H); 3.77-3.91 (m, 1H); 2.43 (s, 3H); 1.15 (d, J=6.28 Hz, 6H). m/z (ESI, +ve ion) 380.1 (M+H)+.

Aufarbeitung

  1. wait80° C. for 2 h
  2. waitThe heating was resumed at 75° C. for another 2 h
  3. temperatureThe mixture was cooled to rt
  4. customsome of the TFA was removed in vacuo
  5. additionSat'd NaHCO3 was added slowly until effervescence
  6. extractionThe aqueous phase was extracted with 25% iPrOH in CHCl3+1% NH4OH (3×10 mL)
  7. dry with materialThe combined organic phases were dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe crude product was purified by silica gel chromatography (25 g, eluent: iPrOH (w/10% NH4OH) in CHCl3 0%-10%)

Quellen und Nachweise

ORD-Eintrag
ord-276addc45f2d4f88843b5a3aff6429c0
Quelldatensatz
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08362241B2

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