Nitric Acid → HCID 601959, 화합물

HRID 613163노트

반응식

HRID 613163 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 601959HCID 601959, 화합물수율 36%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매2회

실험 절차

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.

후처리

  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)]

출처 및 근거

ORD 기록
ord-5894a401a6954071ac51a37c6c9867a9
출처 데이터셋
uspto-grants-1999_12
특허 번호
USRE036477

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