تفاعل #9217

معادلة التفاعل

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

KOH

DMF MeOH

→

desired compound

المردود 15.3%

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

المردود 15.3%

المذيبات

2/1

heptane

MeOH

ظروف التفاعل

المعالجة

1. 1
   أخرىthe precipitation
2. 2
   ترشيحwas filtered off
3. 3
   تركيزThe mother liquid was concentrated
4. 4
   أخرىpurified by prep HPLC

الإجراء التجريبي

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.

المصدر