Реакция #47911

Уравнение реакции

6-Benzyl-5,6,7,8-tetrahydro-N-(4-(trifluoromethylsulfonyl)phenyl)pyrido[4,3-d]pyrimidin-4-amine

1-chloroethylchloroformate

N,N-diisopropylethylamine

→

product

Выход 83.0%

5,6,7,8-Tetrahydro-N-(4-(trifluoromethylsulfonyl)phenyl)pyrido[4,3-d]pyrimidin-4-amine

Выход 83.0%

Растворители

chloroform

Условия реакции

Обработка

1. 1
   workup.STIRRINGthe mixture was stirred for an additional 2 h
2. 2
   ДругоеThe chloroform was removed under vacuum and 30 ml of methanol
3. 3
   workup.ADDITIONwas added
4. 4
   Температураthe mixture was heated for 30 min
5. 5
   ДругоеUpon reaction completion
6. 6
   Другоеthe methanol was removed
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
8. 8
   Промывкаwashed with sat. NaHCO3 and brine
9. 9
   СушкаThe organic layer was dried over Na2SO4
10. 10
    Фильтрацияfiltered
11. 11
    Другоеevaporated

Методика

6-Benzyl-5,6,7,8-tetrahydro-N-(4-(trifluoromethylsulfonyl)phenyl)pyrido[4,3-d]pyrimidin-4-amine (270 mg, 0.55 mmol) was dissolved in anhydrous chloroform (10 mL) and 1-chloroethylchloroformate was added (0.18 mL, 1.65 mmol). After stirring for 30 min, N,N-diisopropylethylamine was added (0.24 mL, 1.65 mmol) and the mixture was stirred for an additional 2 h. The chloroform was removed under vacuum and 30 ml of methanol was added and the mixture was heated for 30 min. Upon reaction completion, the methanol was removed and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give the product (163 mg, 83%).

Источник