Hydrochloric Acid → 1-(3-(1-(5-Chloro-2,3-dimethoxyphenyl)ethylamino)-4-(methylsulfonyl)phenyl)-N,N-dimethylpiperidin-4-amine hydrochloride

HRID 2426074Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2426074
[Cl:1][C:2]1[CH:3]=[C:4]([O:32][CH3:33])[C:5]([O:30][CH3:31])=[C:6]([CH:8]([NH:10][C:11]2[CH:12]=[C:13]([N:21]3[CH2:26][CH2:25][CH:24]([N:27]([CH3:29])[CH3:28])[CH2:23][CH2:22]3)[CH:14]=[CH:15][C:16]=2[S:17]([CH3:20])(=[O:19])=[O:18])[CH3:9])[CH:7]=1.Cl>ClCCl.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([O:32][CH3:33])[C:5]([O:30][CH3:31])=[C:6]([CH:8]([NH:10][C:11]2[CH:12]=[C:13]([N:21]3[CH2:26][CH2:25][CH:24]([N:27]([CH3:28])[CH3:29])[CH2:23][CH2:22]3)[CH:14]=[CH:15][C:16]=2[S:17]([CH3:20])(=[O:19])=[O:18])[CH3:9])[CH:7]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 587072651-(3-(1-(5-chloro-2,3-dimethoxyphenyl)ethylamino)-4-(methylsulfonyl)phenyl)-N,N-dimethylpiperidin-4-amine

Produkt 1

HCID 671473931-(3-(1-(5-Chloro-2,3-dimethoxyphenyl)ethylamino)-4-(methylsulfonyl)phenyl)-N,N-dimethylpiperidin-4-amine hydrochlorideAusbeute 200 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 1-(3-(1-(5-chloro-2,3-dimethoxyphenyl)ethylamino)-4-(methylsulfonyl)phenyl)-N,N-dimethylpiperidin-4-amine (25.0 mg, 0.05 mmol) in dichloromethane (1 mL) was added 0.06 mL (0.06 mmol) of 1 M HCl in diethyl ether. The solution was allowed to stir for 15 minutes and the solvent was removed by rotary evaporation. The residue was dissolved in dichloromethane and triturated with diethyl ether. The solvent was removed by rotary evaporation to collect the title compound (26.0 mg, 0.05 mmol) in 97% yield. 1H NMR (400 MHz, CD3OD): δ 7.49 (d, 1H), 6.93 (s, 1H), 6.91 (s, 1H), 6.37 (d, 1H), 6.08 (s, 1H), 3.93 (m, 2H), 3.90 (s, 3H), 3.86 (s, 3H), 3.45 (m, 1H), 3.04 (s, 3H), 2.92 (m, 2H), 2.82 (s, 6H), 2.04 (t, 2H), 1.66 (m, 2H), 1.55 (d, 3H), 1.49 (m, 2H); MS (ESI) m/z: 497.2 (M++1).

Aufarbeitung

  1. customthe solvent was removed by rotary evaporation
  2. dissolutionThe residue was dissolved in dichloromethane
  3. customtriturated with diethyl ether
  4. customThe solvent was removed by rotary evaporation

Quellen und Nachweise

ORD-Eintrag
ord-98d907f2974d49a9ace75703d3546b0f
Quelldatensatz
uspto-grants-2011_06
Patentnummer
US07968538B2

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