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

HRID 1910632ノート

反応式

HRID 1910632 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fc0514098a3d4029ab8d4a02898091f0
出典データセット
uspto-grants-2013_12
特許番号
US08604021B2

反応ノート

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