Triethylamine → HCID 178446146, Verbindung

HRID 1664545Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1664545
[CH2:1]([N:6]1[C:14]2[N:13]=[CH:12][NH:11][C:10]=2[C:9](=[O:15])[NH:8]/[C:7]/1=[N:16]\[NH2:17])[CH2:2][CH2:3][CH2:4][CH3:5].[Br:18][C:19]1[CH:20]=[C:21]([CH2:25][C:26](O)=[O:27])[CH:22]=[CH:23][CH:24]=1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.C(N(CC)CC)C>CN(C=O)C.CCOC(C)=O>[Br:18][C:19]1[CH:20]=[C:21]([CH2:25][C:26]([NH:17]/[N:16]=[C:7]2\[NH:8][C:9](=[O:15])[C:10]3[NH:11][CH:12]=[N:13][C:14]=3[N:6]\2[CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])=[O:27])[CH:22]=[CH:23][CH:24]=1

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 74653(3-Bromophenyl)acetic acidHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 178446164HCID 178446164, Verbindung

Produkt 1

HCID 178446146HCID 178446146, VerbindungAusbeute 78,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

The mixture of (2E)-3-pentyl-3,7-dihydro-1H-purine-2,6-dione 2-hydrazone (0.30 g, 1.3 mmol), (3-bromophenyl)acetic acid (0.30 g, 1.4 mmol), benzotriazol-1-yloxytris-(dimethylamino)phosphonium hexafluorophosphate (0.62 g, 1.4 mol) and triethylamine (0.53 mL, 3.8 mmol) in DMF (10 mL) were stirred at rt overnight. The reaction mixture was diluted with EtOAc. The solid was filtered, washed with EA and dried to yield the desired product (430 mg, 78.2%). LCMS calculated for C18H22BrN6O2 (M+H): 433.1. found: 433.1.

Aufarbeitung

  1. filtrationThe solid was filtered
  2. washwashed with EA
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d551d0b205e0404eaaff6c9c161aa777
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08039478B2

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