Dimethylformamide → 7-Chloro-9-(1-chloroethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

HRID 626825Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 626825
N1C(Cl)=NC(Cl)=NC=1[Cl:3].[Cl:10][C:11]1[CH:12]=[C:13]([CH:24](O)[CH3:25])[C:14]2[O:20][CH2:19][CH2:18][NH:17][C:16](=[O:21])[C:15]=2[C:22]=1[CH3:23].CN(C)C=O>C(Cl)Cl>[Cl:10][C:11]1[CH:12]=[C:13]([CH:24]([Cl:3])[CH3:25])[C:14]2[O:20][CH2:19][CH2:18][NH:17][C:16](=[O:21])[C:15]=2[C:22]=1[CH3:23]

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 7954Cyanuric chlorideHCID 866975197-Chloro-9-(1-hydroxyethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

Produkt 1

HCID 866975207-Chloro-9-(1-chloroethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-oneAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A mixture of cyanuric chloride (15 mg, 0.079 mmol), 7-chloro-9-(1-hydroxyethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (14 mg, 0.053 mmol) and N,N-dimethylformamide (20 μL) in methylene chloride (0.4 mL) was stirred at room temperature overnight. The mixture was diluted with methylene chloride, washed with saturated sodium bicarbonate, water, brine, dried over sodium sulfate, filtered and concentrated to give the desired compound (10 mg, 70%).

Aufarbeitung

  1. washwashed with saturated sodium bicarbonate, water, brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-4540b44b21964430bed0a6c1e28e027a
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09309251B2

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