反応 #64689

ord-b94fb2c2aa4547d582d45a9b25ab0e89

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared
  2. 2
    温度cooled down
  3. 3
    その他After separation the chloroform phase
  4. 4
    その他was evaporated under reduced pressure
  5. 5
    その他to give a white crystalline product

実験手順

After adding 2.5 ml of the mixture of formic acid and triethylamine prepared according to Example 1 to 2.94 g (0.01 mol) of 5-(3,4-dimethoxyphenylmethyl)-2,2-dimethyl-1,3-dioxane-4,6-dione (m.p.: 142°-144° C.), the reaction mixture was heated to 100° C. for 2 hours, then cooled down. After the addition of 25 ml of water the pH value was adjusted to 1 by adding concentrated hydrochloric acid, then the mixture was thoroughly shaken with 100 ml of chloroform. After separation the chloroform phase was evaporated under reduced pressure to give a white crystalline product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05414108uspto-grants-1995_05