Acetone → HCID 23697072、化合物

HRID 2068002ノート

反応式

HRID 2068002 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 23697072HCID 23697072、化合物収率 101.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-16cc4349b324424487aa1cf4f126e3ad
出典データセット
uspto-grants-2012_10
特許番号
US08293919B2

反応ノート

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