Reaktion #970731

Reaktionsgleichung

Ethyl cyanoacetate

Sodium methoxide

3-methoxypropylthiourea

→

title compound

Ausbeute 48.3%

6-Amino-1-(3-methoxypropyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one

Ausbeute 48.3%

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe resulting white slurry was heated
2. 2
   Temperaturto reflux for 2.5 h
3. 3
   SonstigeThe solvent was evaporated
4. 4
   workup.ADDITIONthe remaining pale brown oil was treated with 2M acetic acid (15 mL)
5. 5
   FiltrationThe white crystals were filtered off
6. 6
   Waschenwashed with acetic acid

Vorschrift

Sodium methoxide (0.81 g, 21.2 mmol, 1.05 eq.) was added to a solution of 3-methoxypropylthiourea (3.00 g, 20.2 mmol) in ethanol (10 mL). Ethyl cyanoacetate (2.18 mL, 20.2 mmol) in ethanol (10 mL) was added and the resulting white slurry was heated to reflux for 2.5 h. The solvent was evaporated and the remaining pale brown oil was treated with 2M acetic acid (15 mL). The white crystals were filtered off and washed with acetic acid to give the title compound (2.10 g, 48%).

Quelle