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

HRID 1390528

反応式

HRID 1390528 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 21731147Trimethylsilylmethyl 2-fluoro-2,2-dinitroethyl ether収率 45%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-49eb490e0b2144e0a3dc99e2a1ca30ec
出典データセット
uspto-grants-1979_02
特許番号
US04139403

関連ノート

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