Reaktion #1904

Reaktionsgleichung

2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone

sodium borohydride

→

2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol

Ausbeute 94.5%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe mixture was concentrated in vacuo
2. 2
   workup.ADDITIONThe residue was diluted with water (200 ml)
3. 3
   Extraktionextracted with ethyl acetate (300 ml)
4. 4
   WaschenThe extract was washed with water
5. 5
   Trocknendried over magnesium sulfate
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)

Vorschrift

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.).

Quelle