Carbon Tetrachloride → Trimethylsilylmethyl 2-fluoro-2,2-dinitroethyl ether

HRID 1390528

반응식

HRID 1390528 반응식
C(=O)([O-])[O-].[K+].[K+].FC(F)(F)S([O:12][CH2:13][Si:14]([CH3:17])([CH3:16])[CH3:15])(=O)=O.[F:20][C:21]([N+:27]([O-:29])=[O:28])([N+:24]([O-:26])=[O:25])[CH2:22]O.C(Cl)(Cl)(Cl)Cl>C(Cl)Cl>[F:20][C:21]([N+:27]([O-:29])=[O:28])([N+:24]([O-:26])=[O:25])[CH2:22][O:12][CH2:13][Si:14]([CH3:15])([CH3:16])[CH3:17]

참가 물질

6

반응물 4

HCID 5943Carbon TetrachlorideHCID 11430Potassium CarbonateHCID 28189Ethanol, 2-fluoro-2,2-dinitro-HCID 2760857(Trimethylsilyl)methyl Trifluoromethanesulfonate [Trimethylsilylmethylating Reagent]

생성물 1

HCID 21731147Trimethylsilylmethyl 2-fluoro-2,2-dinitroethyl ether수율 45%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Potassium carbonate (6 g) was added to a solution of 3.5 g (0.0148 mol) of trimethylsilylmethyl trifluoromethanesulfonate and 2.3 g of 2-fluoro-2,2-dinitroethanol in 5 ml of methylene chloride, and the mixture was stirred for 16 hrs. This suspension was added with stirring to a mixture of 30 ml of ice water and 30 ml of carbon tetrachloride. The carbon tetrachloride layer was washed with 10 ml of water, dried over magnesium sulfate, and distilled to give 1.56 g (45%) of trimethylsilylmethyl 2-fluoro-2,2-dinitroethyl ether, bp 52° (0.75 mm).

후처리

  1. additionThis suspension was added
  2. washThe carbon tetrachloride layer was washed with 10 ml of water
  3. dry with materialdried over magnesium sulfate
  4. distillationdistilled

출처 및 근거

ORD 기록
ord-49eb490e0b2144e0a3dc99e2a1ca30ec
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04139403

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