반응 #9217

반응 방정식

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

KOH

DMF MeOH

→

desired compound

수율 15.3%

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

수율 15.3%

용매

2/1

heptane

MeOH

반응 조건

후처리

1. 1
   기타the precipitation
2. 2
   여과was filtered off
3. 3
   농축The mother liquid was concentrated
4. 4
   기타purified by prep HPLC

실험 절차

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.

출처