反应详情

温度

80 °C

A mixture of tert-butyl 3-[1-(6-benzyloxy-7-fluoro-2-iodo-3-quinolylmethyl)-2-oxo-1,2-dihydro-4-pyridinyl]-3-hydroxypentanoate (obtained according to 1.i, 1.6 g, 2.4 mmol), tetrabutylammonium bromide (0.77 g, 2.4 mmol), potassium acetate (0.24 ml, 2.4 mmol) and palladium acetate (0.55 g, 2.4 mmol) in anhydrous amyl alcohol (30 ml) is heated at 80° C. under an argon atmosphere for 3 hours, then concentrated under reduced pressure. The residue is taken up in methanol (50 ml) and dichloromethane (100 ml), filtered through celite then concentrated under reduced pressure in order to produce a pink solid which is taken up in methanol, then treated with hot activated carbon. The liquor obtained by filtration is concentrated to 5 ml, then placed at 4° C. for 16 hours. The resulting precipitate is collected by filtration and washed with diethyl ether in order to produce, after drying, 370 mg (29%) of a white solid, m.p. >275° C.

1. concentrationconcentrated under reduced pressure
2. filtrationdichloromethane (100 ml), filtered through celite
3. concentrationthen concentrated under reduced pressure in order
4. customto produce a pink solid which
5. additiontreated with hot activated carbon
6. customThe liquor obtained by filtration
7. concentrationis concentrated to 5 ml
8. filtrationThe resulting precipitate is collected by filtration
9. washwashed with diethyl ether in order
10. customto produce
11. customafter drying