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

Trifluoroacetic acid → HCID 86713606, Verbindung

HRID 2274233
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2274233
[CH3:1][C:2]1[C:3]([N:28]2[CH2:33][CH2:32][N:31]([C:34]([O:36]C(C)(C)C)=O)[CH2:30][CH2:29]2)=[N:4][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15](=[O:24])[NH:16][CH:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)=[CH:11][C:10]=2[N+:25]([O-:27])=[O:26])=[N:6][CH:7]=1.C(O)(C(F)(F)F)=O.CC1C(N2CCNCC2)=NC([NH:55][C:56]2[CH:71]=[CH:70][C:59]([C:60]([NH:62]C3CCN(C)CC3)=O)=[CH:58][C:57]=2[N+]([O-])=O)=NC=1.N(C1C=CC(C#N)=CC=1)=C=O.C(N(CC)CC)C>C(Cl)Cl>[C:60]([C:59]1[CH:70]=[CH:71][C:56]([NH:55][C:34]([N:31]2[CH2:32][CH2:33][N:28]([C:3]3[C:2]([CH3:1])=[CH:7][N:6]=[C:5]([NH:8][C:9]4[CH:14]=[CH:13][C:12]([C:15](=[O:24])[NH:16][CH:17]5[CH2:18][CH2:19][N:20]([CH3:23])[CH2:21][CH2:22]5)=[CH:11][C:10]=4[N+:25]([O-:27])=[O:26])[N:4]=3)[CH2:29][CH2:30]2)=[O:36])=[CH:57][CH:58]=1)#[N:62]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 1703804-Cyanophenyl isocyanateHCID 86713605HCID 86713605, VerbindungHCID 86713607HCID 86713607, Verbindung

Produkt 1

HCID 86713606HCID 86713606, Verbindung
Ausbeute 222 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of tert-butyl 4-(5-methyl-2-((4-((1-methylpiperidin-4-yl)carbamoyl)-2-nitrophenyl)amino)pyrimidin-4-yl)piperazine-1-carboxylate (0.073 g, 0.13 mmol) in DCM (1.0 mL) was added TFA (1.0 mL) and the mixture was stirred for 1 h. An aliquot of the reaction mixture was analyzed by LCMS, which indicated that the reaction had proceeded to completion. The solvents were removed and the residue was dried on high vacuum. The crude product was used for the next step without further purification. To a solution of 4-((5-methyl-4-(piperazin-1-yl)pyrimidin-2-yl)amino)-N-(1-methylpiperidin-4-yl)-3-nitrobenzamide (0.073 mmol) in DCM (1.5 mL) was added 4-isocyanatobenzonitrile (23 mg, 0.16 mmol) and triethylamine (0.055 mL, 0.39 mmol) and the mixture was stirred at 23° C. for 16 h. reaction. The crude reaction mixture was filtered and washed with minimal volume of DCM and then hexanes to give the title compound (97 mg, 100%). MS (ES+) C30H34N10O4 requires: 598. Found: 599 [M+H]+

Aufarbeitung

  1. customThe solvents were removed
  2. customthe residue was dried on high vacuum
  3. customThe crude product was used for the next step without further purification
  4. stirringthe mixture was stirred at 23° C. for 16 h.
  5. customreaction
  6. customThe crude reaction mixture
  7. filtrationwas filtered
  8. washwashed with minimal volume of DCM

Quellen und Nachweise

ORD-Eintrag
ord-12386279396449118e4db9c27187f7b4
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09126951B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion