* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With Tris(3,6-dioxaheptyl)amine; potassium carbonate; In dichloromethane; water; for 17h;Heating / reflux;
The compound from step A (6.2 g, 33.5 mmole), (1,3-dioxolan-2-yl-methyl)triphenylphosphonium bromide (22.6 g, 52.7 mmole), tris[2-(2-methoxyethoxy)ethyl]amine (11.2 ml, 34.9 mmole), sat. aq. K2CO3 (150 mls), and CH2Cl2 (150 ml) were heated at reflux for 17 hours. The mixture was cooled and the aqueous layer was washed with CH2Cl2 (2×). The combined organic layers were washed with NaHCO3, brine, dried (MgSO4), and concentrated.
A mixture of NaH (11.3 mmol, 2.0 eq) and ylide salt (11.3 mmol, 2.0 eq) was stirred at 0 C for 1h under N2 protection. Then <strong>[52351-75-4]6-methoxyindoline-2,3-dione</strong> (5.6 mmol, 1.0 eq) was added and the mixture was stirred under 80 C for 2h. The resulting solution was poured into satd.aq. NH4Cl, and the organic layer was separated and dried over Na2SO4. The solvent was removed under reduced pressure and the product was dissolved in CH3CN, follwed by DMAP (11.3 mmol, 2.0 eq), (Boc)2O (11.3 mmol, 2.0eq) were added, the mixture was stirred under room temperature for 20 min. The crude product product was also obtained after the solvent was removed under reduced pressure and then dissloved in EA and stirred with Pd/C (20% w/w) under H2 condition for 4h under room temperature. The mixture was filtered and purified by silica gel chromatography (petroleum ether/ethyl acetate = 8/1-5/1) to afford the product 1t.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
