反应详情

To a solution of 1-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]piperazin-2-one, hydrochloride (0.10 g, 0.267 mmol) and triethylamine (160 μL, 1.148 mmol) in DCM (1.5 mL) is added dropwise ethyl carbonochloridate (35 μL, 0.366 mmol) at room temperature and the reaction mixture is stirred for 1.5 h. The reaction is poured into water and extracted with DCM. After separation, the organic layer is dried over sodium sulphate, filtered and concentrated in vacuo. The residue is purified on silica gel (10 g Isolute cartridge), eluting with EtOAc, to afford a very dense pale yellow oil, which solidified upon addition of Et2O. The material is triturated in Et2O, filtered off and washed twice with Et2O, to afford the title compound (0.066 g, 0.161 mmol) as a colorless solid. MS (m/z) 410 (M+1).

1. extractionextracted with DCM
2. customAfter separation
3. dry with materialthe organic layer is dried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue is purified on silica gel (10 g Isolute cartridge)
7. washeluting with EtOAc
8. customto afford a very dense pale yellow oil, which
9. customThe material is triturated in Et2O
10. filtrationfiltered off
11. washwashed twice with Et2O