反应详情

温度

90 °C

A degassed suspension of the product of Step 1 (50.3 g, 156 mmol), n-Bu4NCl (86.0 g, 312 mmol), LiOAc.2H2O (41.2 g, 390 mmol), LiCl (6.84 g, 156 mmol), Pd(OAc)2 (1.00 g, 4.7 mmol), and methyl 2-iodobenzoate (41.00 g, 156 mmol) in DMF (300 mL) was stirred for 3 hours at 90° C. The dark red solution was then cooled to r.t. and poured into 2 L of ice cold H2O. The product was extracted with hot EtOAc, dried over Na2SO4, filtered and concentrated to dryness. It was dissolved in 600 ml of hot toluene and filtered through a small silica pad (1 L). The title product was finally recrystallized from EtOAc:hexane 1:1 (1.2 L). The title product was finally recrystallized from EtOAc:hexane 1:1 (1.2 L). Recrystallization of the mother liquors in EtOAc:hexane 1:3 ( 400 mL) afforded a second crop of the title compound.

1. temperatureThe dark red solution was then cooled to r.t.
2. extractionThe product was extracted with hot EtOAc
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. dissolutionIt was dissolved in 600 ml of hot toluene
7. filtrationfiltered through a small silica pad (1 L)
8. customThe title product was finally recrystallized from EtOAc:hexane 1:1 (1.2 L)
9. customThe title product was finally recrystallized from EtOAc:hexane 1:1 (1.2 L)
10. customRecrystallization of the mother liquors in EtOAc:hexane 1:3 ( 400 mL)