Reaktion #996565

Reaktionsgleichung

product

4-[4-(2-Amino-ethoxy)-3-bromo-5-ethoxy-phenyl]-2-methyl-5-oxo-7-propyl-1,4,5,6,7,8-hexahydro-quinoline-3-carbonitrile

triethylamine

methanesulfonyl chloride

→

N-{2-[2-Bromo-4-(3-cyano-2-methyl-5-oxo-7-propyl-1,4,5,6,7,8-hexahydroquinolin-4-yl)-6-ethoxy-phenoxy]-ethyl}-methanesulfonamide

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with 0.5N aqueous HCl
2. 2
   TrocknenThe organic layer was dried (MgSO4)
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated in vacuo
5. 5
   SonstigeThe residue was purified by preparative HPLC (Method B)

Vorschrift

A mixture of the product of step c (130.7 mg), triethylamine (93 μl) and methanesulfonyl chloride 21 μl in dichloromethane (3 ml) was stirred for 17 h. The mixture was diluted with dichloromethane and washed with 0.5N aqueous HCl. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by preparative HPLC (Method B). Yield: 57.1 mg. MS-ESI: [M+H]+=566.0/568.0; HPLC: Rt=12.49 min. (method 1). Diast. ratio: 4:1

Quelle