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 1910589노트

반응식

HRID 1910589 반응식
[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

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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%)

출처 및 근거

ORD 기록
ord-3ddacbc5b35c4c938eb21c63726d912a
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604021B2

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