반응 #433262

ord-0c60fc9c7d2d4369bc4e91d6229ef8fa

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 16 hours
  2. 2
    온도refluxing
  3. 3
    여과The solid was filtered
  4. 4
    세척washed with water
  5. 5
    기타dried
  6. 6
    기타recrystallised from acetic acid
  7. 7
    기타to give the product (49.0 g, 77.2% theory) as a white crystalline solid, mpt 150°-153° C. (98.2% pure by hplc)

실험 절차

6-Hydroxynaphthalene-2-carboxylic acid (39.8 g), 1-bromooctane (61.3 g), potassium hydroxide (23.7 g), ethanol (900 ml) and water (120 ml) were stirred and refluxed for 16 hours. 10% Aqueous potassium hydroxide (200 ml) was added and refluxing was continued for a further 2 hours, when the solution was poured into water (5 liter) and acidified to ph 1. The solid was filtered, washed with water, dried and recrystallised from acetic acid to give the product (49.0 g, 77.2% theory) as a white crystalline solid, mpt 150°-153° C. (98.2% pure by hplc).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05061399uspto-grants-1991_10