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Dimethyl Sulfoxide → 2-Pyrimidineacetic acid ethyl ester

HRID 1907676
ノート
印刷プレビュー

反応式

HRID 1907676 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[CH:7](C(OCC)=O)[C:8]([O:10][CH2:11][CH3:12])=[O:9].CS(C)=O.[Cl-].[Na+]>O>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 2303274Diethyl (pyrimidin-2-yl)propanedioate

生成物 1

HCID 123671052-Pyrimidineacetic acid ethyl ester収率 63.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
142.5 °C

実験手順

4.76 g of diethyl (2-pyrimidinyl)malonate and 20 ml of dimethyl sulfoxide were mixed. To the mixture was added 1.40 g of sodium chloride and 0.72 g of water. The mixture was stirred for about 20 minutes at an inner temperature of 140 to 145° C., and for about 20 minutes at an inner temperature of 145 to 148° C. The mixture was allowed to cool to room temperature, then, to the reaction mixture was added water, and extracted with ethyl acetate. The organic layer was washed with saturated brine twice, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure to obtain 2.12 g of ethyl (2-pyrimidinyl)acetate.

後処理

  1. waitfor about 20 minutes at an inner temperature of 145 to 148° C
  2. temperatureto cool to room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine twice
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5a5fcd2cabd048ffb1528e6dd563e24a
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08598176B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート