Hydrochloric Acid → N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride

HRID 1978526Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1978526
[CH3:1][O:2][C:3]([C:5]1[CH:35]=[CH:34][CH:33]=[CH:32][C:6]=1[O:7][CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:13][CH2:12]1)=[O:4].[ClH:36]>C(O)C>[ClH:36].[ClH:36].[CH3:1][O:2][C:3]([C:5]1[CH:35]=[CH:34][CH:33]=[CH:32][C:6]=1[O:7][CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:13][CH2:12]1)=[O:4]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 21993853N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

Produkt 1

HCID 21994086N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochlorideAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 0.81 g (1.64 inmol.) of N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (5 ml) was added, at room temperature, 1 ml (12 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes. The reaction mixture was concentrated, to which was added acetonitrile. The resulting crystalline precipitate was collected by filtration, which was washed with ethanol and diethyl ether to give the object compound (809.1 mg, 87%) as orange crystals, m.p.164-168° C.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated, to which
  2. additionwas added acetonitrile
  3. filtrationThe resulting crystalline precipitate was collected by filtration, which
  4. washwas washed with ethanol and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-ddd33cfa13f24474b2138a130c78f5e8
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06235731B1

Notizen zur Reaktion

Wird geladen…