反应详情

A suspension of PdCl2 (0.15 g) in 2,3-dibromothianaphthene (2.4 g) was brought to the temperature of 115° C., and P(OEt)3 (3.3 g) was then dropped under stirring and in an inert atmosphere. Once dropping was completed, the red solution was brought to 160° C. After 1 h 30 min, the mixture was diluted with CH2Cl2, washed twice with water and dehydrated. The solvent was evaporated at reduced pressure to yield a residue that underwent chromatography on silica gel by flash chromatography (AcOEt), to yield 2,3-bis(diethoxyphosphoryl)-benzo[b]thiophene (1.6 g) (yield 60%).

1. additionwas then dropped
2. customwas brought to 160° C
3. washwashed twice with water
4. customThe solvent was evaporated at reduced pressure
5. customto yield a residue that underwent chromatography on silica gel by flash chromatography (AcOEt)