Sulfuric Acid → Epoxysuccinic acid

HRID 436909

反応式

HRID 436909 の反応式
C([O-])(=O)/C=C\C([O-])=O.[Ca+2].[O:10]1[CH:15]([C:16]([O-:18])=[O:17])[CH:11]1[C:12]([O-:14])=[O:13].[Ca+2].[Ca].S(=O)(=O)(O)O>CC(C)=O>[O:10]1[CH:15]([C:16]([OH:18])=[O:17])[CH:11]1[C:12]([OH:14])=[O:13]

参加物

6

反応物 4

HCID 1118Sulfuric Acid3 回HCID 5460341CalciumHCID 6916005Maleic acid, calcium saltHCID 13538056Calcium epoxysuccinate2 回

生成物 1

HCID 86022Epoxysuccinic acid収率 97%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
50 °C

実験手順

The epoxidation of acid calcium maleate was effected in accordance with Example 1. 50 g. of the calcium epoxysuccinate attained in this manner (calcium content 11.9% by weight) were suspended, with stirring, in 400 g. of 50% aqueous acetone. 15 g. of concentrated sulphuric acid were then added and the suspension was kept for 2 hours at 20° C. If the suspension is made in acetone alone, a corresponding amount of dilute sulphuric acid may be added instead of concentrated sulphuric acid. The suspension was then heated to 50° C. and, after being kept for 2 hours at this temperature, the calcium sulphate was filtered off and washed with water. The acetone was removed by distillation from the mixture of acetone and water, and the remaining aqueous epoxysuccinic acid solution was subjected directly to hydrolysis. From two moles of acid calcium epoxysuccinate, 512 g. of free epoxysuccinic acid were obtained, corresponding to a yield of 97% of the theoretical.

後処理

  1. waitafter being kept for 2 hours at this temperature
  2. filtrationthe calcium sulphate was filtered off
  3. washwashed with water
  4. customThe acetone was removed by distillation from the mixture of acetone and water
  5. customthe remaining aqueous epoxysuccinic acid solution was subjected directly to hydrolysis

出典と根拠

ORDレコード
ord-3ae237c421dd4d15b204a533982db57a
出典データセット
uspto-grants-1977_06
特許番号
US04028407

関連ノート

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