反応 #64716

ord-17e1a6fc8d7f4900b476ff014efbe71c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他obtained in Reference Example 2
  2. 2
    その他The organic layer was separated off
  3. 3
    抽出the aqueous layer was extracted with chloroform
  4. 4
    洗浄the combined organic layer was washed with 2N aqueous hydrochloric acid solution
  5. 5
    乾燥dried over anhydrous magnesium sulfate
  6. 6
    濃縮The resulting solution was concentrated under reduced pressure

実験手順

In 20 ml of methylene chloride were dissolved 1.08 g of 2,4-dimethoxyaniline and 4.5 ml of triethylamine. To this solution was dropwise added under ice cooling 20 ml of methylene chloride containing 3 g of 2-[bis(4-acetoxyphenyl)methyl]benzoyl chloride obtained in Reference Example 2. After stirring for 7 hours, water was added thereto. The organic layer was separated off, and the aqueous layer was extracted with chloroform. The chloroform layer was combined with the organic layer, and the combined organic layer was washed with 2N aqueous hydrochloric acid solution and dried over anhydrous magnesium sulfate. The resulting solution was concentrated under reduced pressure to give 2.6 g of the desired product (Compound 2) as an oily matter.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05413997uspto-grants-1995_05