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Hydrochloric Acid → N-(1-(5-Chloro-2,3-dimethoxyphenyl)ethyl)-5-(4-methylpiperazin-1-yl)-2-(methylsulfonyl)benzenamine hydrochloride

HRID 2426072
ノート
印刷プレビュー

反応式

HRID 2426072 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([O:30][CH3:31])[C:5]([O:28][CH3:29])=[C:6]([CH:8]([NH:10][C:11]2[CH:16]=[C:15]([N:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)[CH:14]=[CH:13][C:12]=2[S:24]([CH3:27])(=[O:26])=[O:25])[CH3:9])[CH:7]=1.Cl>ClCCl.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([O:30][CH3:31])[C:5]([O:28][CH3:29])=[C:6]([CH:8]([NH:10][C:11]2[CH:16]=[C:15]([N:17]3[CH2:18][CH2:19][N:20]([CH3:23])[CH2:21][CH2:22]3)[CH:14]=[CH:13][C:12]=2[S:24]([CH3:27])(=[O:25])=[O:26])[CH3:9])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 58707275N-(1-(5-chloro-2,3-dimethoxyphenyl)ethyl)-5-(4-methylpiperazin-1-yl)-2-(methylsulfonyl)benzenamine

生成物 1

HCID 67147329N-(1-(5-Chloro-2,3-dimethoxyphenyl)ethyl)-5-(4-methylpiperazin-1-yl)-2-(methylsulfonyl)benzenamine hydrochloride収率 180%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of N-(1-(5-chloro-2,3-dimethoxyphenyl)ethyl)-5-(4-methylpiperazin-1-yl)-2-(methylsulfonyl)benzenamine (45.1 mg, 0.10 mmol) in dichloromethane (2 mL) was added 0.06 mL (0.13 mmol) of 2 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 (43.0 mg, 0.09 mmol) in 89.6% yield. 1H NMR (400 MHz, CD3OD): δ 7.51 (d, 1H), 6.92 (m, 2H), 6.36 (d, 1H), 6.10 (s, 1H), 4.94 (m, 1H), 3.92 (m, 4H), 3.89 (s, 3H), 3.86 (s, 3H), 3.49 (m, 2H), 3.11 (m, 2H), 3.04 (s, 3H), 2.90 (s, 3H), 1.56 (d, 3H); MS (ESI) m/z: 468.0 (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-9b3995ebf6454dbba4b72602a403a863
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07968538B2

反応ノート

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