反应详情

温度

70 °C

A solution of 15.6 g of 1 (62 mmol) in 300 ml of THF was added 30 g of 10% Pd-C, 40 g of ammonium formate and 17.2 ml of triethyl amine. The reaction mixture was heated at 70° C. for 6 hours and filtered. The filtrate was concentrated and redissolved in 500 ml of ethyl acetate and washed with 2×150 ml of 3% aqueous HCl and 2×100 ml of brine. The organic layer was concentrated and triturated with 1:1 ethyl acetate:hexane to give 8 g (31.2 mmol, 51%) of 2.

1. filtrationfiltered
2. concentrationThe filtrate was concentrated
3. dissolutionredissolved in 500 ml of ethyl acetate
4. washwashed with 2×150 ml of 3% aqueous HCl and 2×100 ml of brine
5. concentrationThe organic layer was concentrated
6. customtriturated with 1:1 ethyl acetate