反応 #9229

反応方程式

1-(6-phenylacetylenyl-2-benzothiazolyl)-3-ethylurea

→

desired compound

収率 41.0%

1-(6-(2(Z)-Phenylvinyl)-2-benzothiazolyl)-3-ethylurea

収率 41.0%

溶媒

ethanol

反応条件

後処理

1. 1
   その他was purged with nitrogen gas
2. 2
   その他by bubbling of hydrogen gas
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他purified by preparative TLC

実験手順

A suspension of 1-(6-phenylacetylenyl-2-benzothiazolyl)-3-ethylurea (0.032 g, 83% purity by weight, 0.083 mmol) and Lindlar catalyst (0.030 g, 5% weight purity, 0.012 mmol, 0.15 eq) in 2 mL ethanol was purged with nitrogen gas, followed by bubbling of hydrogen gas. It was stirred under hydrogen atmosphere for about 36 hours. The mixture was taken up in 10 mL MeOH, filtered, concentrated, and purified by preparative TLC to give 0.011 g (41%) of the desired compound. LC/MS 324 (M+1); LC retention time 2.84 min.

出典