Sodium → 3-methoxy-4-thioacetoxy-2E-butenoic acid methyl ester

HRID 1165083

反応式

HRID 1165083 の反応式
[Na].[C:2]([OH:5])(=[S:4])[CH3:3].[CH3:6][O:7][C:8](=[O:15])/[CH:9]=[C:10](/[O:13][CH3:14])\[CH2:11]Cl>CO>[CH3:6][O:7][C:8](=[O:15])/[CH:9]=[C:10](/[O:13][CH3:14])\[CH2:11][O:5][C:2](=[S:4])[CH3:3]

参加物

5

反応物 3

HCID 5360545SodiumHCID 6364655Methyl (E)-4-Chloro-3-methoxy-2-butenoateHCID 178418634HCID 178418634、化合物

生成物 1

HCID 1317163333-methoxy-4-thioacetoxy-2E-butenoic acid methyl ester収率 98.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
0 °C

実験手順

4.07 g (0.177 mol) of sodium is dissolved in 180 ml of methanol and cooled to 0° C. 13.47 g (0.171 mol) of thioacetic acid is instilled in this solution. Then this solution is mixed at 0° C. with a solution of 29.15 g (0.150 mol) of 3-methoxy-4-chloro-2E-butenoic acid methyl ester in 40 ml of methanol. It is stirred again overnight at room temperature. The precipitated salt is filtered off, the solvent is evaporated on the rotary evaporator and mixed with a little methylene filtering off, evaporation of the solvent and drying of the residue in a high vacuum, 36.53 g of a yellow-colored liquid with a content according to GC of 82.8 percent is obtained. This corresponds to 30.25 g of 100 percent product=98.7 percent yield. Further data concerning the compound is:

後処理

  1. filtrationThe precipitated salt is filtered off
  2. customthe solvent is evaporated on the rotary evaporator
  3. additionmixed with a little methylene filtering off,
  4. customevaporation of the solvent
  5. dry with materialdrying of the residue in a high vacuum, 36.53 g of a yellow-colored liquid with a content
  6. customis obtained

出典と根拠

ORDレコード
ord-07bd276e3fe0492fbd6f12c5a5889d40
出典データセット
uspto-grants-1990_03
特許番号
US04906765

関連ノート

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