Sodium Sulfite → Sodium 2-chlorobenzene-1-sulfinate

HRID 1944446노트

반응식

HRID 1944446 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 23719078Sodium 2-chlorobenzene-1-sulfinate수율 97.8%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
75 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ce1e75f48d66433b9b338dc893c648cd
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394836B2

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