反应详情

温度

100 °C

To a mixture of 14.6 g (60.5 mmol) of 4-bromo-1-methoxy-2-methylindane, 10.8 g (60.5 mmol) of 1-methoxy-2-methyl-4-indanol, 38.5 g (181 mmol) K3PO4, and 200 ml of toluene, a mixture of 696 mg (1.21 mmol) Pd(dba)2 and 825 mg (2.42 mmol) of 2-di(tert-butyl)phosphino-2′-(N,N-dimethylamino)biphenyl was added under an argon atmosphere. This mixture was stirred for 14 hours at 100° C. Then, 300 ml of water was added. The organic layer was separated, and the aqueous layer was extracted with 3×100 ml of CH2Cl2. The combined extract was washed with 2×100 ml of water, dried over K2CO3, and evaporated to dryness. The analytically pure product was obtained using flash chromatography on Silica Gel 60 (40-63 μm, d 50 mm, l 400 mm, eluant: hexanes-dichloromethane=1:1, vol.). Yield, 12.4 g (61%). On the evidence of NMR spectra, the product consists of a mixture of isomers.

1. additionwas added under an argon atmosphere
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with 3×100 ml of CH2Cl2
4. extractionThe combined extract
5. washwas washed with 2×100 ml of water
6. dry with materialdried over K2CO3
7. customevaporated to dryness
8. customThe analytically pure product was obtained
9. customYield
10. additionOn the evidence of NMR spectra, the product consists of a mixture of isomers