Reaktion #9217

Reaktionsgleichung

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

KOH

DMF MeOH

→

desired compound

Ausbeute 15.3%

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

Ausbeute 15.3%

Lösungsmittel

2/1

heptane

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe precipitation
2. 2
   Filtrationwas filtered off
3. 3
   EinengenThe mother liquid was concentrated
4. 4
   Sonstigepurified by prep HPLC

Vorschrift

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.

Quelle