반응 #1377878

ord-fd4eff7937b14029a33cc68d8338781d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과after which the resulting solid was collected by vacuum filtration
  2. 2
    세척washed with 2×100 ml of ethyl ether
  3. 3
    workup.DISSOLUTIONThe solid was dissolved in 200 ml of water
  4. 4
    여과The resulting precipitate was collected by vacuum filtration
  5. 5
    세척washed with 200 ml water
  6. 6
    기타dried overnight in vacuo at 30° C

실험 절차

To a 500 ml erlenmeyer flask with magnetic stirrer was charged 10.3 g of 3-nitro4-methoxy-methylbenzoate, 400 ml tetrahydrofuran, and 3.2 g of 86% potassium hydroxide. The reaction was stirred for 12 hours at ambient temperature, after which the resulting solid was collected by vacuum filtration and washed with 2×100 ml of ethyl ether. The solid was dissolved in 200 ml of water and acidified to pH 4 with 6N hydrochloric acid. The resulting precipitate was collected by vacuum filtration, washed with 200 ml water, and dried overnight in vacuo at 30° C. Isolated 7.4 g of product as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05753642uspto-grants-1998_05