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

HRID 2426074노트

반응식

HRID 2426074 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-98d907f2974d49a9ace75703d3546b0f
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968538B2

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