反応 #5972

ord-4563d094e20d4ff7b79cc94364998fa9

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度This is cooled
  2. 2
    その他the methanol is removed under vacuo
  3. 3
    workup.ADDITIONdiluted with 30 ml water
  4. 4
    ろ過filtered
  5. 5
    抽出extracted with ethyl acetate
  6. 6
    洗浄washed with water
  7. 7
    乾燥dried over magnesium sulfate
  8. 8
    その他evaporated to dryness
  9. 9
    その他to give crystalline product which

実験手順

A mixture of 1.6 g of methyl 2-chloro-5a,6,7, 8,9,9a-hexahydrodibenzofuran-4-carboxylate in 10 ml of methanol and 20 ml of 1N sodium hydroxide is stirred at 50° C. for 6 hours. This is cooled, the methanol is removed under vacuo, diluted with 30 ml water and filtered. The aqueous solution is acidified with acetic acid, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and evaporated to dryness to give crystalline product which is used directly in the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246942uspto-grants-1993_09