Nitric Acid → HCID 601959、化合物

HRID 613163ノート

反応式

HRID 613163 の反応式
[CH3:1][Si:2]([CH3:14])([CH3:13])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Si](C)(C)C)[CH:4]=1.[N+:15]([O-])([OH:17])=[O:16].C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>C(OC(=O)C)(=O)C>[N+:15]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([Si:2]([CH3:14])([CH3:13])[CH3:1])[CH:4]=1)([O-:17])=[O:16]

参加物

6

反応物 4

HCID 944Nitric AcidHCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 12358188(1,3-Phenylene)bis(trimethylsilane)

生成物 1

HCID 601959HCID 601959、化合物収率 36%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒2 回

実験手順

To a solution of 1.50 g (6.75 mmol) of m-bis(trimethylsilyl)benzene in 4.0 ml of acetic anhydride was added dropwise a solution of 1.6 ml (35.6 mmol) of 94% nitric acid in 5 ml of acetic anhydride at 130° C. with stirring. The mixture was stirred for 30 minutes. The reaction mixture was poured into a mixture of ice and 2% potassium carbonate solution and methylene chloride and separated. The aqueaus layer was extracted with methylene chloride. The organic layer was washed successively with water and 2% potassium hydroxide solution, dried and evaporated. The residue was purified by column chromatography on silica gel [eluent: methylene chloride-cyclohexane (1:3-1:5)] to give 475 mg of pale yellow liquid.

後処理

  1. stirringThe mixture was stirred for 30 minutes
  2. customseparated
  3. extractionThe aqueaus layer was extracted with methylene chloride
  4. washThe organic layer was washed successively with water and 2% potassium hydroxide solution
  5. customdried
  6. customevaporated
  7. customThe residue was purified by column chromatography on silica gel [eluent: methylene chloride-cyclohexane (1:3-1:5)]

出典と根拠

ORDレコード
ord-5894a401a6954071ac51a37c6c9867a9
出典データセット
uspto-grants-1999_12
特許番号
USRE036477

反応ノート

読み込み中…