Sulfuryl chloride → 4-Chloro-2-(n-propoxyimino)acetoacetic acid methyl ester

HRID 465239ノート

反応式

HRID 465239 の反応式
[CH3:1][O:2][C:3](=[O:13])[C:4](=[N:8][O:9][CH2:10][CH2:11][CH3:12])[C:5]([CH3:7])=[O:6].S(Cl)([Cl:17])(=O)=O>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:13])[C:4](=[N:8][O:9][CH2:10][CH2:11][CH3:12])[C:5]([CH2:7][Cl:17])=[O:6]

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 54207568HCID 54207568、化合物

生成物 1

HCID 542547764-Chloro-2-(n-propoxyimino)acetoacetic acid methyl ester収率 94%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
40 °C

実験手順

To a solution of 7.4 g of 2-(n-propoxyimino)acetoacetic acid methyl ester in 7.4 ml of acetic acid is added 5.5 g of sulfuryl chloride, and the mixture is stirred for 10 minutes at 40° C., then for 6 hours at room temperature. The reaction solution is poured into 100 ml of ice-water, and subjected to extraction twice with chloroform. The extract is washed with an aqueous solution of sodium chloride, and aqueous solution of sodium bicarbonate and water in this order, and dried over anhydrous sodium sulfate. The solvent is evaporated under reduced pressure to yield 8.2 g (94%) of 4-chloro-2-(n-propoxyimino)acetoacetic acid methyl ester as a pale yellow oil product.

後処理

  1. waitfor 6 hours at room temperature
  2. extractionsubjected to extraction twice with chloroform
  3. washThe extract is washed with an aqueous solution of sodium chloride, and aqueous solution of sodium bicarbonate and water in this order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-e9b2a9d1200241148ead4cf12478f210
出典データセット
uspto-grants-1985_10
特許番号
US04550105

反応ノート

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