反応 #6977

反応方程式

sodium ethoxide

ethyl-6-amino-nicotinate

benzoyl isothiocyanate

→

6-thioureido-nicotinic acid ethyl ester

収率 77.0%

溶媒

ethanol

THF

反応条件

後処理

1. 1
   その他the volatiles were removed in vacuo
2. 2
   その他the solid formed
3. 3
   ろ過was collected by filtration
4. 4
   洗浄rinsed with water
5. 5
   その他dried

実験手順

A mixture of ethyl-6-amino-nicotinate (2.5 g, 15 mmol) and benzoyl isothiocyanate (2.45 g, 15 mmol) in THF (20 mL) was heated at 40° C. for 4 h. To this mixture at RT, was added sodium ethoxide (2.04 g, 30 mmol) in ethanol (10 mL). After stirring the resulting mixture at RT for 16 h, the volatiles were removed in vacuo. The residue was suspended in aqueous NH4Cl and the solid formed was collected by filtration, rinsed with water and dried to afford 6-thioureido-nicotinic acid ethyl ester as a white solid (2.6 g, 77% yield). LC/MS; (M+H)+=226.

出典