反応 #67692

反応方程式

3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid amide

N,N′-dimethylethylenediamine

5-bromo-9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalene

K2CO3

→

3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid (9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-yl)-amide

反応条件

後処理

1. 1
   その他A 20 ml screw-cap vial
2. 2
   workup.ADDITIONwas filled with the following solids
3. 3
   workup.ADDITIONA magnetic stir bar was added
4. 4
   その他the open vial was gently flushed with N2
5. 5
   workup.ADDITIONDioxane (2 mL) was added
6. 6
   その他The vial was sealed
7. 7
   その他placed into a preheated screening block at 130° C
8. 8
   その他The yield (HPLC-analysis) of the compound of formula I

実験手順

A 20 ml screw-cap vial was filled with the following solids: CuO (0.05 mmol, 4.0 mg), anhydrous CuCl2 (0.05 mmol, 6.7 mg), K2CO3 (2.0 mmol, 277 mg), 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid amide (1.1 mmol, 193 mg) and 5-bromo-9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalene (1.0 mmol, 304 mg). A magnetic stir bar was added, and the open vial was gently flushed with N2. Dioxane (2 mL) was added, followed by N,N′-dimethylethylenediamine (0.45 mmol, 48 μl). The vial was sealed and placed into a preheated screening block at 130° C. Conversion was complete after 24 hours. The yield (HPLC-analysis) of the compound of formula I was 70%.

出典