Sodium Sulfite → Sodium 2-chlorobenzene-1-sulfinate

HRID 1944446ノート

反応式

HRID 1944446 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8](Cl)(=[O:10])=[O:9].O1CCOCC1.C(=O)(O)[O-].[Na+:22].S([O-])([O-])=O.[Na+].[Na+]>O>[Na+:22].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([O-:10])=[O:9]

参加物

6

反応物 4

HCID 24437Sodium SulfiteHCID 312751,4-DioxaneHCID 761872-Chlorobenzenesulfonyl chlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 23719078Sodium 2-chlorobenzene-1-sulfinate収率 97.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
75 °C

実験手順

A mixture of 2-chlorobenzenesulfonyl chloride (2.5 g) and dioxane (35 mL) was treated with a mixture of sodium bicarbonate (2.0 g), sodium sulfite (3.0 g) and water (17 mL), and the resulting mixture was heated at 75° C. for 30 minutes. The mixture was cooled to room temperature and concentrated under reduced pressure. The residue was triturated with ethanol, filtered and the filtrate concentrated under reduced pressure. The residue was triturated with acetonitrile to afford the title compound as a white solid (2.3 g).

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was triturated with ethanol
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customThe residue was triturated with acetonitrile

出典と根拠

ORDレコード
ord-ce1e75f48d66433b9b338dc893c648cd
出典データセット
uspto-grants-2013_03
特許番号
US08394836B2

反応ノート

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