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

HRID 127887ノート

反応式

HRID 127887 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 354.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Trichloroethyl pyruvate (3.7 g, 1.7 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-d3d5be830ce9495da8661c047a363561
出典データセット
uspto-grants-1981_03
特許番号
US04257947

反応ノート

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