反応 #328198

反応方程式

2-amino-5-bromopyridine

ethoxycarbonylisothiocyanate

→

ethyl {[(5-bromopyridin-2-yl)amino]carbonothioyl}carbamate

収率 70.3%

溶媒

dioxane

反応条件

後処理

1. 1
   濃縮The mixture was then concentrated
2. 2
   その他the residue triturated with 10% ethyl acetate in hexanes
3. 3
   ろ過The solid was collected by filtration
4. 4
   その他dried

実験手順

To a solution of 2-amino-5-bromopyridine (5.0 g, 29 mmol) in dioxane (60 mL) was added ethoxycarbonylisothiocyanate (3.4 mL, 29 mmol) in a dropwise manner and the mixture was allowed to stir for 18 h at room temperature. The mixture was then concentrated and the residue triturated with 10% ethyl acetate in hexanes. The solid was collected by filtration and dried to afford ethyl {[(5-bromopyridin-2-yl)amino]carbonothioyl}carbamate (6.2 g, 69%) as a colorless solid. MS (EI) for C9H10BrN3O2S: 305 (MH+).

出典