Pyridine → N-{3-Chloro-4-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]phenyl}propane-2-sulfonamide

HRID 2414325

Reaktionsgleichung

Reaktionsgleichung von HRID 2414325
[CH:1]([S:4](Cl)(=[O:6])=[O:5])([CH3:3])[CH3:2].[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[CH2:24][O:23][C:22]3=[O:31])[CH2:17][CH2:16]2)=[C:11]([Cl:32])[CH:10]=1.N1C=CC=CC=1>C(#N)C>[Cl:32][C:11]1[CH:10]=[C:9]([NH:8][S:4]([CH:1]([CH3:3])[CH3:2])(=[O:6])=[O:5])[CH:14]=[CH:13][C:12]=1[N:15]1[CH2:20][CH2:19][CH:18]([N:21]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][O:23][C:22]2=[O:31])[CH2:17][CH2:16]1

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 824082-Propanesulfonyl chlorideHCID 226446801-[1-(4-Amino-2-chlorophenyl)piperidin-4-yl]-1,4-dihydro-2H-3,1-benzoxazin-2-one

Produkt 1

HCID 22644580N-{3-Chloro-4-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]phenyl}propane-2-sulfonamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Isopropylsulphonyl chloride (0.03 ml) was added to a stirred solution of the product from example 120 step (ii) (0.05 g), pyridine (0.1 ml) in acetonitrile (0.9 ml) at room temperature. The mixture was stirred overnight, partitioned between ethyl acetate and water, the organics separated, washed with water, dried, and evaporated under reduced pressure. Purification was by chromatography eluting with 40% ethyl acetate/isohexane. Yield 0.015 g.

Aufarbeitung

  1. custompartitioned between ethyl acetate and water
  2. washthe organics separated, washed with water
  3. customdried
  4. customevaporated under reduced pressure
  5. customPurification
  6. washeluting with 40% ethyl acetate/isohexane

Quellen und Nachweise

ORD-Eintrag
ord-558892f7f8eb43d7a45a1efaf662520b
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06812226B2

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