Reaktion #41835

Reaktionsgleichung

(4-morpholin-4-ylmethyl-phenyl)-piperazin-1-yl-methanone

(1-ethoxy-cyclopropoxy)-trimethyl-silane

acetic acid

NaBH3CN

→

title compound

(4-Cyclopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas cooled to room temperature
2. 2
   Einengenconcentrated
3. 3
   workup.ADDITIONThe residue was diluted with 1 N NaOH
4. 4
   Extraktionextracted with CH2Cl2
5. 5
   TrocknenThe organic layer was dried (Na2SO4)
6. 6
   Einengenconcentrated
7. 7
   SonstigeThe residue was purified by column chromatography (SiO2)

Vorschrift

A solution of (4-morpholin-4-ylmethyl-phenyl)-piperazin-1-yl-methanone (0.128 g) in methanol (7.5 mL) was treated with (1-ethoxy-cyclopropoxy)-trimethyl-silane (1.5 mL), acetic acid (0.2 mL), and NaBH3CN (˜400 mg). The mixture was heated at 60° C. for 18 h, and then was cooled to room temperature and concentrated. The residue was diluted with 1 N NaOH and extracted with CH2Cl2. The organic layer was dried (Na2SO4) and concentrated. The residue was purified by column chromatography (SiO2) to yield the title compound.

Quelle