反应 #1904

ord-8a08d4d95931403fb13cf9932fe3b98e

反应方程式

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
收率 94.5%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩the mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONThe residue was diluted with water (200 ml)
  3. 3
    萃取extracted with ethyl acetate (300 ml)
  4. 4
    洗涤The extract was washed with water
  5. 5
    干燥dried over magnesium sulfate
  6. 6
    浓缩concentrated in vacuo
  7. 7
    其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)

实验过程

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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726306uspto-grants-1998_03