反応 #1154656

反応方程式

ammonia

N-(4-cyanophenyl)-glycine

carbonyldiimidazole

1-(4-methylamino-3-aminobenzyl)-2-methyl-benzimidazole

→

2-(4-cyanophenylaminomethyl)-1-methyl-5-[(2-methylbenzimidazol-1-yl)methyl]-benzimidazole

溶媒

water

tetrahydrofuran

反応条件

後処理

1. 1
   温度is refluxed for a further 16 hours
2. 2
   その他Then the solution is evaporated to dryness
3. 3
   workup.ADDITIONthe residue is mixed with 80 ml glacial acetic acid
4. 4
   温度refluxed for 1 hour
5. 5
   その他It is then evaporated to dryness once more
6. 6
   その他the residue thus obtained
7. 7
   その他The product which crystallises out is suction
8. 8
   ろ過filtered
9. 9
   洗浄washed with a little water
10. 10
    その他dried

実験手順

A mixture of 1.94 g (11.0 mmol) of N-(4-cyanophenyl)-glycine and 1.78 g (11.0 mmol) of carbonyldiimidazole is refluxed in 80 ml of absolute tetrahydrofuran for 15 minutes. After the addition of 2.7 g (10.46 mmol) of 1-(4-methylamino-3-aminobenzyl)-2-methyl-benzimidazole the mixture is refluxed for a further 16 hours. Then the solution is evaporated to dryness, the residue is mixed with 80 ml glacial acetic acid and refluxed for 1 hour. It is then evaporated to dryness once more, the residue thus obtained is mixed with 50 ml of water and made alkaline with conc. ammonia (about pH 10). The product which crystallises out is suction filtered, washed with a little water and dried.

出典