反应详情

To a solution of triphosgene (30 mg, 0.1 mmol) in dry DCM (1 ml) at CPC, under nitrogen atmosphere, DIPEA (0.175 ml, 1.0 mmol) was added followed by the addition (slowly added) of a solution of 6-(7-methylspiro[2H-benzofuran-3,1′-cyclopropane]-4-yl)oxypyridin-3-amine (Intermediate 158, 27 mg, 0.1 mmol) in dry DCM (2 ml) and the reaction mixture was stirred for 15 minutes at the same temperature. After that a solution of Methyl 2-amino-2-methylpropanoate hydrochloride (30 mg, 0.2 mmol) in dry DCM (2 ml) was added and the reaction mixture was stirred for 30 minutes at 0° C. The reaction was quenched with a 1M aqueous solution of HCl (5 ml), diluted with DCM (10 ml) and two phases were separated. The organic layer was washed with brine (10 ml), dried (Na2SO4), filtered and evaporated affording the urea intermediate as yellow foam.

1. additionfollowed by the addition (
2. stirringthe reaction mixture was stirred for 30 minutes at 0° C
3. customThe reaction was quenched with a 1M aqueous solution of HCl (5 ml)
4. additiondiluted with DCM (10 ml) and two phases
5. customwere separated
6. washThe organic layer was washed with brine (10 ml)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customevaporated