Reacción #9217

Ecuación de reacción

1-(7-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea

KOH

DMF MeOH

→

desired compound

Rendimiento 15.3%

1-(7-Acetylenyl-2-benzothiazolyl)-3-ethylurea

Rendimiento 15.3%

Disolventes

2/1

heptane

MeOH

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe precipitation
2. 2
   Filtraciónwas filtered off
3. 3
   ConcentraciónThe mother liquid was concentrated
4. 4
   Otropurified by prep HPLC

Procedimiento

A mixture of 1-(7-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea 2 (0.050 g, 0.16 mmol) and 1M aqueous KOH solution (0.16 mL, 0.16 mmol, 1.0 eq) in 1.5 mL of 2/1 mixture of DMF/MeOH was stirred at room temperature for about 2 hours. The mixture was taken up in 10 mL MeOH and the precipitation was filtered off. The mother liquid was concentrated and purified by prep HPLC to give the desired compound 0.006 g (15%). LC/MS 246 (M+1); LC retention time 2.77 min.

Fuente