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Trifluoroacetic acid → N-(5-amino-2-methylphenyl)-4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamide

HRID 1465030
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1465030
[CH:1]1([NH:4][C:5]2[C:6]3[S:13][CH:12]=[C:11]([C:14]([NH:16][C:17]4[CH:18]=[C:19]([NH:24]C(=O)OC(C)(C)C)[CH:20]=[CH:21][C:22]=4[CH3:23])=[O:15])[C:7]=3[N:8]=[CH:9][N:10]=2)[CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:24][C:19]1[CH:20]=[CH:21][C:22]([CH3:23])=[C:17]([NH:16][C:14]([C:11]2[C:7]3[N:8]=[CH:9][N:10]=[C:5]([NH:4][CH:1]4[CH2:2][CH2:3]4)[C:6]=3[S:13][CH:12]=2)=[O:15])[CH:18]=1
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Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 67361287t-Butyl 3-(4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamido)-4-methylphenylcarbamate

Produkt 1

HCID 67360673N-(5-amino-2-methylphenyl)-4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

t-Butyl 3-(4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamido)-4-methylphenylcarbamate (7 g, 15.93 mmol) was dissolved in DCM (80 mL), TFA (12 mL, 159.3 mmol) was added thereto, and the mixture was stirred at room temperature for 8 hours. After the reaction was completed, the reaction mixture was concentrated under reduced pressure to remove the organic solvent and the remaining TFA, and water (20 mL) was added thereto. The reaction mixture was neutralized with 2.0 N NaOH solution, and the resulting yellow solid was filtered and dried to obtain the title compound without further purification.

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customto remove the organic solvent
  3. additionthe remaining TFA, and water (20 mL) was added
  4. filtrationthe resulting yellow solid was filtered
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e0c046fd91ce4bc289aba9f8c6b97a85
Quelldatensatz
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08999973B2

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