反应详情

温度

60 °C

A solution of 85 mg (0.35 mMol) 6-amino-4-(1,2,3,4-tetrahydro-quinolin-6-yloxy)-pyrimidine (Step 1.3) and 0.33 mMol (4-pyrrolidin-1-ylmethyl-3-trifluoromethyl-phenyl)-carbamic acid phenyl ester in 2 ml DMSO is heated to 60° C. Then 65 μl (0.38 mMol) diisopropyl-ethyl-amine are added and stirring at 60° C. continued for 3 h. The resulting solution is poured into water containing 30 mg KOH and EtOAc, the aqueous layer separated off and extracted 2× with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; EtOAC→EtOAc/(EtOH+1.5% Et3N) 19:1) gives the title compound: MS: [M+1]+=513; HPLC: tARet=8.8; Anal.: C,H,N,F.

1. customthe aqueous layer separated off
2. extractionextracted 2× with EtOAc
3. washThe organic phases are washed with water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated