Ammonia → 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide

HRID 515483Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 515483
[C:1]1([C@H:7]([N:9]2[CH2:15][CH2:14][CH:13]([C:16]3[CH:24]=[CH:23][C:19]([C:20](O)=[O:21])=[CH:18][CH:17]=3)[O:12][CH2:11][CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.N.[Cl-].COC1N=C(OC)N=C([N+]2(C)CCOCC2)[N:32]=1>CN(C)C=O.O>[C:1]1([C@H:7]([N:9]2[CH2:15][CH2:14][CH:13]([C:16]3[CH:24]=[CH:23][C:19]([C:20]([NH2:32])=[O:21])=[CH:18][CH:17]=3)[O:12][CH2:11][CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 887MethanolHCID 27340594-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chlorideHCID 672831054-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzoic acid

Produkt 1

HCID 672820504-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzoic acid (diastereomer type A) (0.96 g, 2.9 mmol) and 7 mol/L methanol solution of ammonia (2 mL, 14 mmol) in N,N-dimethylformamide (10 mL) was added 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (1.25 g, 4.5 mmol) at room temperature and the mixture was stirred for one day. The reaction mixture was poured into water. The resulting white solid material was collected by filtration and dried under reduced pressure at 50° C. for 5 hours to yield 4-[4-((R)-1-phenyl-ethyl)-[1,4]oxazepan-7-yl]-benzamide (diastereomer type A) (0.58 g, 1.78 mmol, 61%).

Aufarbeitung

  1. filtrationThe resulting white solid material was collected by filtration
  2. customdried under reduced pressure at 50° C. for 5 hours

Quellen und Nachweise

ORD-Eintrag
ord-a77b7ebc592a4110b3d193610203c98a
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108957B2

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