反応 #165803

反応方程式

(benzotriazol-1-yloxy-dimethylamino-methylene)-dimethyl-ammonium tetrafluoroborate

4-[5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl]-N,N-dimethyl-benzamide

6-aminopyridine-2-carboxylic acid

triethylamine

→

4-(5-amino-6-(2-(6-aminopyridine-2-carbonyl)hydrazinecarbonyl)pyrazin-2-yl)-N,N-dimethylbenzamide

溶媒

DMF

反応条件

後処理

1. 1
   温度then warmed slightly
2. 2
   workup.ADDITIONThe mixture was poured dropwise onto water (5 ml) with rapid stirring
3. 3
   workup.STIRRINGstirred at room temperature for 1 h
4. 4
   ろ過then filtered
5. 5
   その他to give a wet paste which
6. 6
   その他was dried under high vacuum at 100° C. overnight
7. 7
   その他Used directly in the next step without purification

実験手順

A solution of 4-[5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl]-N,N-dimethyl-benzamide (100 mg, 0.3163 mmol) and 6-aminopyridine-2-carboxylic acid (43.69 mg, 0.3163 mmol) in DMF (1.000 mL) was treated with triethylamine (32.01 mg, 44.09 μL, 0.3163 mmol) then warmed slightly. The mixture was cooled to room temperature and then treated with (benzotriazol-1-yloxy-dimethylamino-methylene)-dimethyl-ammonium tetrafluoroborate (121.9 mg, 0.3796 mmol) and stirred at room temperature overnight. The mixture was poured dropwise onto water (5 ml) with rapid stirring, stirred at room temperature for 1 h then filtered to give a wet paste which was dried under high vacuum at 100° C. overnight. Used directly in the next step without purification.

出典