Hydrochloric Acid → N-(1-(6-Chloro-2,3-dihydrobenzo[b][1,4]dioxin-8-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine hydrochloride

HRID 1910589ノート

反応式

HRID 1910589 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([CH:12]([NH:14][C:15]2[CH:20]=[C:19]([N:21]3[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)[CH:18]=[CH:17][C:16]=2[S:27]([CH3:30])(=[O:29])=[O:28])[CH3:13])[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[CH:3]=1.Cl>ClCCl.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:11]=[C:10]([CH:12]([NH:14][C:15]2[CH:20]=[C:19]([N:21]3[CH2:22][CH2:23][NH:24][CH2:25][CH2:26]3)[CH:18]=[CH:17][C:16]=2[S:27]([CH3:30])(=[O:29])=[O:28])[CH3:13])[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[CH:3]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 11633830N-(1-(6-chloro-2,3-dihydrobenzo[b][1,4]dioxin-8-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine

生成物 1

HCID 67147366N-(1-(6-Chloro-2,3-dihydrobenzo[b][1,4]dioxin-8-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of N-(1-(6-chloro-2,3-dihydrobenzo[b][1,4]dioxin-8-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine (50.0 mg, 0.11 mmol) in anhydrous dichloromethane (1 mL) was cooled to 0° C. and HCl (0.12 mL of a 1 M solution in diethyl ether, 0.12 mmol) was added. The mixture was allowed to stir for 30 min. The solvent was removed by rotary evaporation, more diethyl ether was added to precipitate the salt. After removal of solvent by rotary evaporation the desired product was collected (53 mg, 99%). 1H NMR (400 MHz, CD3OD): δ 7.55 (d, 1H), 6.87 (d, 1H), 6.76 (d, 1H), 6.40 (dd, 1H), 6.02 (d, 1H), 4.84 (m, 1H), 4.33 (m, 2H), 4.27 (m, 2H), 4.43 (m, 4H), 3.30 (m, 4H), 3.07 (s, 3H), 1.54 (d, 3H); MS (ESI) m/z: 452.3 (M++1).

後処理

  1. customThe solvent was removed by rotary evaporation, more diethyl ether
  2. additionwas added
  3. customto precipitate the salt
  4. customAfter removal of solvent
  5. customby rotary evaporation the desired product
  6. customwas collected (53 mg, 99%)

出典と根拠

ORDレコード
ord-3ddacbc5b35c4c938eb21c63726d912a
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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