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

HRID 33789

反応式

HRID 33789 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
125 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-10fa31c5cc2749d2a1fbbb1cd161dbd5
出典データセット
uspto-grants-2008_09
特許番号
US07429660B2

関連ノート

読み込み中…