Реакция #2448606

Уравнение реакции

9-(2-methyl-3-(4-oxoquinazolin-3(4H)-yl)phenyl)-2-trityl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole-6-carboxamide

EtOAc

HCl

→

desired product

Выход 90.0%

9-(2-Methyl-3-(4-oxoquinazolin-3(4H)-yl)phenyl)-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole-6-carboxamide

Выход 90.0%

Растворители

methanol

Условия реакции

Обработка

1. 1
   Другоеto form a clear solution
2. 2
   Другоеforming a cloudy mixture which
3. 3
   Концентрированиеthe mixture was concentrated under vacuum
4. 4
   workup.ADDITIONtreated with NaHCO3 (aq) and EtOAc
5. 5
   workup.STIRRINGstirred at room temperature for about 1 h
6. 6
   ФильтрацияThe precipitate was collected by filtration
7. 7
   Промывкаwashed with water
8. 8
   Сушкаwith EtOAc, and dried under vacuum

Методика

A suspension of 9-(2-methyl-3-(4-oxoquinazolin-3(4H)-yl)phenyl)-2-trityl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indole-6-carboxamide (248.5 mg, 0.359 mmol) in methanol (4 mL) was treated with EtOAc (less than 1 mL) to form a clear solution. This was treated with 1 M aqueous HCl (3 mL), forming a cloudy mixture which was stirred at room temperature. After 30 min, the mixture was concentrated under vacuum, treated with NaHCO3 (aq) and EtOAc and stirred at room temperature for about 1 h. The precipitate was collected by filtration, washed with water, then with EtOAc, and dried under vacuum to provide the desired product as a white solid (145 mg, 90% yield).

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