Acetone → HCID 23697072, 화합물

HRID 2068002노트

반응식

HRID 2068002 반응식
S([O-])([O-])=O.[Na+:5].[Na+].CC(C)=O.[CH3:11][C:12]1[C:16]([S:17](Cl)(=[O:19])=[O:18])=[C:15]([CH3:21])[O:14][N:13]=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH3:11][C:12]1[C:16]([S:17]([O-:19])=[O:18])=[C:15]([CH3:21])[O:14][N:13]=1.[Na+:5]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 10340Sodium CarbonateHCID 24437Sodium SulfiteHCID 27363193,5-Dimethylisoxazole-4-sulfonyl chloride

생성물 1

HCID 23697072HCID 23697072, 화합물수율 101.1%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
80 °C

실험 절차

A solution of sodium sulfite (680 mg, 5.40 mmol) in water (5 mL) was added to an acetone (5 mL) solution of 3,5-dimethylisoxazole-4-sulfonyl chloride (530 mg, 2.70 mmol). The mixture was heated to 80° C., then a solution of sodium carbonate (430 mg, 4.05 mmol) in water (5 ml) was added dropwise. The mixture was refluxed for 16 hours then evaporated to dryness. The residue was refluxed with ethanol (20 mL), the inorganics were removed by filtration. Evaporation of the filtrate afforded 500 mg of crude sodium 3,5-dimethylisoxazole-4-sulfinate. It was used in the next steps without further purification. 1H NMR (400 MHz, DMSO-d6): δ 2.37 (s, 3H) and 2.22 (s, 3H).

후처리

  1. temperatureThe mixture was refluxed for 16 hours
  2. customthen evaporated to dryness
  3. temperatureThe residue was refluxed with ethanol (20 mL)
  4. customthe inorganics were removed by filtration
  5. customEvaporation of the filtrate

출처 및 근거

ORD 기록
ord-16cc4349b324424487aa1cf4f126e3ad
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293919B2

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