Nitric Acid → Stattic

HRID 554246

反応式

HRID 554246 の反応式
[N+:1]([O-:4])(O)=[O:2].[S:5]1(=[O:15])(=[O:14])[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH:7]=[CH:6]1>S(=O)(=O)(O)O>[N+:1]([C:11]1[CH:12]=[CH:13][C:8]2[CH:7]=[CH:6][S:5](=[O:15])(=[O:14])[C:9]=2[CH:10]=1)([O-:4])=[O:2]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 69997Benzothiophene 1,1-dioxide

生成物 1

HCID 2779853Stattic収率 84%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

Nitric acid (10 mL) was slowly added to sulfuric acid (10 mL) at 0° C., and the mixture was stirred at the same temperature for 10 min. To this solution was slowly added 1-benzothiophene 1,1-dioxide (3.99 g) at 0° C., and the mixture was further stirred at the same temperature for 30 min. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The extract was washed twice with water, saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give the title compound as a pale-yellow solid (yield 4.26 g, 84%).

後処理

  1. customat 0° C.
  2. stirringthe mixture was further stirred at the same temperature for 30 min
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed twice with water, saturated aqueous sodium hydrogencarbonate solution and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-e4f3bb9c71194648a0196fccda63007a
出典データセット
uspto-grants-2011_11
特許番号
US08048909B2

関連ノート

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