반응 #1904

ord-8a08d4d95931403fb13cf9932fe3b98e

반응 방정식

COc1cc(OCc2ccccc2)ccc1C(=O)c1cc(Cl)ccc1N
2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone
[BH4-].[Na+]
sodium borohydride
COc1cc(OCc2ccccc2)ccc1C(O)c1cc(Cl)ccc1N
2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol
수율 94.5%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThe residue was diluted with water (200 ml)
  3. 3
    추출extracted with ethyl acetate (300 ml)
  4. 4
    세척The extract was washed with water
  5. 5
    건조dried over magnesium sulfate
  6. 6
    농축concentrated in vacuo
  7. 7
    기타The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726306uspto-grants-1998_03