반응 #47911

반응 방정식

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

1-chloroethylchloroformate

N,N-diisopropylethylamine

→

product

수율 83.0%

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

수율 83.0%

용매

chloroform

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred for an additional 2 h
2. 2
   기타The chloroform was removed under vacuum and 30 ml of methanol
3. 3
   workup.ADDITIONwas added
4. 4
   온도the mixture was heated for 30 min
5. 5
   기타Upon reaction completion
6. 6
   기타the methanol was removed
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
8. 8
   세척washed with sat. NaHCO3 and brine
9. 9
   건조The organic layer was dried over Na2SO4
10. 10
    여과filtered
11. 11
    기타evaporated

실험 절차

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%).

출처