HCID 67199810, Verbindung → HCID 86621654, Verbindung

HRID 547565Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 547565
[ClH:1].[NH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([NH:16]C(=O)C)=[CH:12][CH:11]=2)[CH:6]=[C:5]([CH3:20])[N:4]=1>Cl>[ClH:1].[NH2:16][C:13]1[CH:12]=[CH:11][C:10]([NH:9][C:7]2[CH:6]=[C:5]([CH3:20])[N:4]=[C:3]([NH2:2])[N:8]=2)=[CH:15][CH:14]=1

Komponenten

3

Edukt 1

HCID 67199810HCID 67199810, Verbindung

Produkt 1

HCID 86621654HCID 86621654, VerbindungAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

To a suspension of 16 (6.0 g, 20 mmol) was added 2N HCl (40 mL) and the mixture was refluxed for 20 h. The solvents were evaporated to dryness, residue boiled in MeOH and diluted with EtOAc. The resulting precipitate was filtered and washed with EtOAc and dried to give essentially pure 17 (5.0 g, 97%); mp (MeOH/EtOAc) 275-280° C.; 1H NMR [(CD3)2SO] δ 12.50 (br, 1 H, N+H), 10.75 (br s, 1 H, NH), 9.75 (br s, 2 H, NH2), 7.85 (br s, 4 H, NH2 & ArH)), 7.34 (d, J=8.6 Hz, 2 H, ArH), 6.24 (br s, 1 H, ArH), 2.79 (s, 3 H, CH3), HRMS (FAB+) calc. for C11H14N5 (M+1) m/z 216.1249, found 216.1247.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 20 h
  2. customThe solvents were evaporated to dryness, residue
  3. additiondiluted with EtOAc
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with EtOAc
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-dc63f2df74344b81bdaad353d1faac06
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07939546B2

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