Sulfuric Acid → 1-[3-(1H-benzo[d]imidazol-2-yl)-4-chlorophenyl]piperidin-4-one

HRID 2047380

Reaktionsgleichung

Reaktionsgleichung von HRID 2047380
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[CH:11]=[C:12]([N:17]2[CH2:26][CH2:25][C:20]3(OCC[O:21]3)[CH2:19][CH2:18]2)[CH:13]=[CH:14][C:15]=1[Cl:16].OS(O)(=O)=O.C([O-])([O-])=O.[Na+].[Na+]>O>[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[CH:11]=[C:12]([N:17]2[CH2:26][CH2:25][C:20](=[O:21])[CH2:19][CH2:18]2)[CH:13]=[CH:14][C:15]=1[Cl:16]

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 595680638-[3-(1H-benzoimidazol-2-yl)-4-chloro-phenyl]-1,4-dioxa-8-aza-spiro[4.5]decane

Produkt 1

HCID 595682431-[3-(1H-benzo[d]imidazol-2-yl)-4-chlorophenyl]piperidin-4-oneAusbeute 90,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a suspension of 8-[3-(1H-benzoimidazol-2-yl)-4-chloro-phenyl]-1,4-dioxa-8-aza-spiro[4.5]decane (2.00 g, 5.42 mmol) in water (50 mL) was added H2SO4 (2.50 mL) dropwise and the resulting solution was stirred for 72 h at room temperature. The solution was neutralized with Na2CO3 and the oil obtained solidified on standing in water. The precipitate was filtered and dried to obtain 1.60 g (90%) of the title compound.

Aufarbeitung

  1. customthe oil obtained
  2. filtrationThe precipitate was filtered
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-565b7d65a1f1425f9f69c4fbec066c11
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08592463B2

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