Hydrochloric Acid → 2-(2-Bromo-phenylsulfanyl)-5-nitro-benzenesulfinic acid

HRID 33789

반응식

HRID 33789 반응식
[OH-].[Na+].[Br:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[SH:10].Cl[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][C:13]=1[S:21]([OH:23])=[O:22].Cl>O>[Br:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][C:13]=1[S:21]([OH:23])=[O:22]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 805982-BromobenzenethiolHCID 1115232-Chloro-5-nitrobenzenesulphinic acid

생성물 1

HCID 597974372-(2-Bromo-phenylsulfanyl)-5-nitro-benzenesulfinic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
125 °C

실험 절차

To a solution of NaOH (80.18 g, 2.004 mol) in water (600 ml sonicated and degassed) was added 2-bromothiophenol (108.23 ml, 1.002 mol) and 2-chloro-5-nitro-benzenesulfinic acid (222.11 g, 1.002 mol). The mixture was stirred and heated at 125° C. for 19 hours. The reaction was cooled down at 0° C., and concentrated HCl added dropwise from a dropping funnel while stirring until pH<1. The precipitate formed was filtered, dried in a desiccators overnight and was used without any further purification (417.77 g). m/z (LC-MS, ESP), RT=3.51 min, (M−−1)=372-374, (1:1, bromine isotope ratio present).

후처리

  1. temperatureThe reaction was cooled down at 0° C.
  2. stirringwhile stirring until pH<1
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. customdried in a desiccators overnight
  6. customwas used without any further purification (417.77 g)

출처 및 근거

ORD 기록
ord-10fa31c5cc2749d2a1fbbb1cd161dbd5
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

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