Reaktion #87404

Reaktionsgleichung

6-[(Cyclopropylmethoxy)methyl]-2-sulfanylidene-1,2,3,4-tetrahydropyrimidin-4-one

bromoacetic acid

sodium hydroxide

→

title compound

Ausbeute 37.0%

6-[(Cyclopropylmethoxy)methyl]-1,2,3,4-tetrahydropyrimidine-2,4-dione

Ausbeute 37.0%

Lösungsmittel

EtOH

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was refluxed for 16 h
2. 2
   EinengenThe mixture was concentrated in vacuo and hydrochloric acid (aq, 10%)
3. 3
   workup.ADDITIONwas added
4. 4
   SonstigeThe precipitate was isolated by filtration
5. 5
   Sonstigedried

Vorschrift

6-[(Cyclopropylmethoxy)methyl]-2-sulfanylidene-1,2,3,4-tetrahydropyrimidin-4-one (10.3 g, 48.5 mmol) was added to bromoacetic acid (21.5 g, 155 mmol, 3.2 eq) in EtOH (108 mL) and H2O (441 mL). The reaction mixture was refluxed for 16 h then cooled down to rt and basified to pH˜10 with sodium hydroxide (3 M, aq). The mixture was concentrated in vacuo and hydrochloric acid (aq, 10%) was added. The mixture was cooled to 0° C. The precipitate was isolated by filtration and dried to give the title compound as a solid (3.5 g, 37%).

Quelle