反应详情

温度

60 °C

1-Chloroethyl chloroformate (543 mg, 3.8 mmol) was added dropwise to the solution of 7-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4-amine from Example 31 (820 mg, 1.9 mmol) and diisopropylethyl amine (490 mg, 3.8 mmol) in 1,2-dichloroethane (5 mL, anhydrous) at room temperature. After addition, the reaction mixture was stirred at 60° C. for 2 h in the atmosphere of nitrogen. Solvent was removed in vacuo, residue was dissolved in methanol (10 mL) and was stirred at 60° C. for 1 hr. Solvent was removed in vacuo, residue was dissolved in ethyl acetate and was washed by sodium bicarbonate aqueous solution, brine and dried over sodium sulfate. Solvent was removed in vacuo and light orange oily residue was directly taken to the next step.

1. additionAfter addition
2. customSolvent was removed in vacuo, residue
3. dissolutionwas dissolved in methanol (10 mL)
4. stirringwas stirred at 60° C. for 1 hr
5. customSolvent was removed in vacuo, residue
6. dissolutionwas dissolved in ethyl acetate
7. washwas washed by sodium bicarbonate aqueous solution, brine
8. dry with materialdried over sodium sulfate
9. customSolvent was removed in vacuo and light orange oily residue