Carbon Dioxide → 2,2,2-Trichloroethyl 3-bromo-2-oxopropanoate

HRID 1862869ノート

反応式

HRID 1862869 の反応式
[C:1]([O:6][CH2:7][C:8]([Cl:11])([Cl:10])[Cl:9])(=[O:5])[C:2]([CH3:4])=[O:3].[Br:12]Br.C(=O)=O>O>[Br:12][CH2:4][C:2](=[O:3])[C:1]([O:6][CH2:7][C:8]([Cl:9])([Cl:10])[Cl:11])=[O:5]

参加物

5

反応物 3

HCID 280Carbon DioxideHCID 24408BromineHCID 129644372,2,2-Trichloroethyl 2-oxopropanoate

生成物 1

HCID 143497182,2,2-Trichloroethyl 3-bromo-2-oxopropanoate収率 35.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Trichloroethyl pyruvate (3.7 g, 17 mmole) is heated to 65° and 1.1 ml (17 mmole) of bromine is added dropwise over 1 hour. A stream of carbon dioxide is passed through the reaction mixture during the addition to remove the HBr formed in the reaction. The mixture is cooled to room temperature, diluted with water and extracted with ethyl acetate. The extract is dried over MgSO4, evaporated and distilled in vacuum to give 1.8 g of trichloroethyl bromopyruvate, bp 74°-77° (0.01 mm).

後処理

  1. customto remove the HBr
  2. customformed in the reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract is dried over MgSO4
  5. customevaporated
  6. distillationdistilled in vacuum

出典と根拠

ORDレコード
ord-936400cb750543c7b72239f4cd3ddc47
出典データセット
uspto-grants-1979_09
特許番号
US04166816

反応ノート

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