反应详情

130 mg (0.44 mMol) triphosgene are dissolved in 5 ml ice-cooled CH2Cl2. Then a solution of 170 mg (1.12 mMol) adamantan-1-ylamine and 0.5 ml (2.87 mMol) EtN(iPr)2 in 5 ml CH2Cl2 is added during 15 min. After stirring the reaction mixture for further 15 min, a solution of 300 mg (1.33 mMol) 5-(2-amino-pyrimidin-4-yloxy)-2,3-dihydro-1H-indole (Step 26.2) and 0.5 ml (2.87 mMol) EtN(iPr)2 in 5 ml THF is added. After 16 h at rt, the mixture is diluted with 10% NaHCO3 solution and CH2Cl2, the aqueous phase separated off and extracted with CH2Cl2. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; hexane/EtOAc 19:1→3:1) gives the title compound: MS: [M+1]+=406; HPLC: EtRet=3.7.

1. waitAfter 16 h at rt
2. customthe aqueous phase separated off
3. extractionextracted with CH2Cl2
4. washThe organic layers are washed with water and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated