تفاعل #1904

ord-8a08d4d95931403fb13cf9932fe3b98e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزthe mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThe residue was diluted with water (200 ml)
  3. 3
    استخلاصextracted with ethyl acetate (300 ml)
  4. 4
    غسيلThe extract was washed with water
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    تركيزconcentrated in vacuo
  7. 7
    أخرىThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)

الإجراء التجريبي

To a solution of 2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone (10 g) in methanol (100 ml) was added sodium borohydride (1.4 g). After being stirred for 24 h, the mixture was concentrated in vacuo. The residue was diluted with water (200 ml) and extracted with ethyl acetate (300 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1) to give 2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol (9.5 g) as colorless crystals (mp=101°-103° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726306uspto-grants-1998_03