反応 #1607035

反応方程式

Thieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidine-9-carbonitrile

N1-methylethane-1,2-diamine

NH4Cl

→

titled compound

5-Amino-4-(4H-1,2,4-triazol-3-yl)thiophene-3-carbonitrile

溶媒

MeOH

反応条件

後処理

1. 1
   温度immediately cooled in an ice bath
2. 2
   抽出the aqueous mixture was extracted with 10% iPrOH/CHCl3 (3×)
3. 3
   乾燥dried (MgSO4)
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under reduced pressure

実験手順

Thieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidine-9-carbonitrile (251 mg, 1.25 mmol) was dissolved in MeOH (6.2 mL), and N1-methylethane-1,2-diamine (0.22 mL, 2.5 mmol) was added. This was heated to 60° C. for 20 min, then immediately cooled in an ice bath. Saturated NH4Cl (30 mL) was added, then the aqueous mixture was extracted with 10% iPrOH/CHCl3 (3×). The organic layers were combined, dried (MgSO4), filtered and concentrated under reduced pressure to give the titled compound as a single peak on LC/MS: method [4], retention time=0.658 min; MS(ESI) 192.0 (MH+).

出典