StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

4-(2,6-Diamino-pyrimidin-4-yloxy)-benzoic acid hydrazide → 6-{4-[5-(4-chloro-3-trifluoromethyl-phenylamino)-4H-[1,2,4]triazol-3-yl]phenoxy}-pyrimidine-2,4-diamine

HRID 387439
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 387439
[NH2:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:18]=[CH:17][C:12]([C:13]([NH:15][NH2:16])=O)=[CH:11][CH:10]=2)[CH:5]=[C:4]([NH2:19])[N:3]=1.I.CS[C:23](=[NH:36])[NH:24][C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([C:32]([F:35])([F:34])[F:33])[CH:26]=1>N1C=CC=CC=1>[Cl:31][C:28]1[CH:29]=[CH:30][C:25]([NH:24][C:23]2[NH:36][C:13]([C:12]3[CH:17]=[CH:18][C:9]([O:8][C:6]4[N:7]=[C:2]([NH2:1])[N:3]=[C:4]([NH2:19])[CH:5]=4)=[CH:10][CH:11]=3)=[N:15][N:16]=2)=[CH:26][C:27]=1[C:32]([F:33])([F:34])[F:35]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 591353394-(2,6-Diamino-pyrimidin-4-yloxy)-benzoic acid hydrazideHCID 1785040011-[4-chloro-3-(trifluoromethyl)phenyl]-S-methylisothiourea hydroiodide

Produkt 1

HCID 1785079266-{4-[5-(4-chloro-3-trifluoromethyl-phenylamino)-4H-[1,2,4]triazol-3-yl]phenoxy}-pyrimidine-2,4-diamineAusbeute 50,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

4-[(2,6-diaminopyrimidin-4-yl)oxy]benzohydrazide (1.48 g, 5.68 mmol) and S-methyl N-[4-chloro-3-(trifluoromethyl)phenyl]isothiourea hydroiodide (2.33 g, 5.89 mmol) were suspended in 30 mL of anhydrous pyridine. The reaction mixture was refluxed for 18 hours under Ar atmosphere. The formed yellow solution was cooled down to ambient temperature and pyridine was removed in vacuo. The resulting yellow foamy solid was re-dissolved in 50 mL of 5:1 EtOAc/MeOH; ca. 15 g of silica gel was added and solvent was removed in vacuo. The impregnated silica gel was packed into ISCO column and the product was purified using ISCO system (80 g pre-packed column, 50 min run, 0% to 10% gradient of solvent B in solvent A [Solvent A—4 mL of MeOH, 4 ml, of Et3N in 4 L of CH2Cl2; Solvent B—4 mL of Et3N in 4 L of MeOH]). Solvent was removed in vacuo to give the title product as a white solid (1.33 g). Yield 50.5%.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 18 hours under Ar atmosphere
  2. custompyridine was removed in vacuo
  3. dissolutionThe resulting yellow foamy solid was re-dissolved in 50 mL of 5:1 EtOAc/MeOH
  4. additionca. 15 g of silica gel was added
  5. customsolvent was removed in vacuo
  6. customthe product was purified
  7. customISCO system (80 g pre-packed column, 50 min run, 0% to 10% gradient of solvent B in solvent A [Solvent A—4 mL of MeOH, 4 ml, of Et3N in 4 L of CH2Cl2; Solvent B—4 mL of Et3N in 4 L of MeOH])
  8. customSolvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-72f8e43f01ca4a7888db5ee90438059b
Quelldatensatz
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08372971B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion