Реакция #1154656

Уравнение реакции

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

Растворители

water

tetrahydrofuran

Условия реакции

Обработка

1. 1
   Температураis refluxed for a further 16 hours
2. 2
   ДругоеThen the solution is evaporated to dryness
3. 3
   workup.ADDITIONthe residue is mixed with 80 ml glacial acetic acid
4. 4
   Температураrefluxed for 1 hour
5. 5
   ДругоеIt is then evaporated to dryness once more
6. 6
   Другоеthe residue thus obtained
7. 7
   ДругоеThe product which crystallises out is suction
8. 8
   Фильтрацияfiltered
9. 9
   Промывкаwashed with a little water
10. 10
    Другоеdried

Методика

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.

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