Tetrahydrofuran → HCID 178512227, Verbindung

HRID 16158

Reaktionsgleichung

Reaktionsgleichung von HRID 16158
FC(F)(F)C#[N:4].[Cl:7][C:8]1[CH:33]=CC2O[C:13]3[CH:31]=[CH:30]C=C[C:14]=3[C@@H:15]3[C@H:20]([NH:21][C:22](=O)[C:23]([F:26])([F:25])[F:24])[CH2:19][CH2:18][CH2:17][N:16]3[C:10]=2[CH:9]=1.[CH2:34]1[CH2:38][O:37][CH2:36][CH2:35]1>>[Cl:7][C:8]1[CH:33]=[CH:35][C:36]2[O:37][C:38]3[CH:34]=[CH:30][CH:31]=[CH:13][C:14]=3[C@@H:15]3[C@H:20]([NH:21][C:22](=[NH:4])[C:23]([F:26])([F:25])[F:24])[CH2:19][CH2:18][CH2:17][N:16]3[C:10]=2[CH:9]=1

Komponenten

4

Edukt 3

HCID 8028TetrahydrofuranHCID 67710TrifluoroacetonitrileHCID 86599857trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide

Produkt 1

HCID 178512227HCID 178512227, VerbindungAusbeute 55 %

Versuchsvorschrift

Trifluoroacetonitrile was added to a solution of trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (10 mg, 0.03 mmol) in 2 mL of THF for 2 h. The mixture was stirred at room temperature for 16 hr. After evaporation the crude compound was chromatographed on silica. Elution with toluene gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetimidamide (7.14 mg, 55%). Data: (m/z)=396 (M+H)+.

Aufarbeitung

  1. customAfter evaporation the crude compound
  2. customwas chromatographed on silica
  3. washElution with toluene

Quellen und Nachweise

ORD-Eintrag
ord-da440b6bedae44c09fe04691b0dac5a9
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07737136B2

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