反応 #47911

反応方程式

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

1-chloroethylchloroformate

N,N-diisopropylethylamine

→

product

収率 83.0%

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

収率 83.0%

溶媒

chloroform

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred for an additional 2 h
2. 2
   その他The chloroform was removed under vacuum and 30 ml of methanol
3. 3
   workup.ADDITIONwas added
4. 4
   温度the mixture was heated for 30 min
5. 5
   その他Upon reaction completion
6. 6
   その他the methanol was removed
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
8. 8
   洗浄washed with sat. NaHCO3 and brine
9. 9
   乾燥The organic layer was dried over Na2SO4
10. 10
    ろ過filtered
11. 11
    その他evaporated

実験手順

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%).

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