With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7688-25-7,1,4-Bis(diphenylphosphino)butane,as a common compound, the synthetic route is as follows.
10. Preparation of 1-Ethyl-4-(2-chloro-3-(2-methoxyethoxy)-4-methylsulfonylbenzoyl)-5-hydroxypyrazole from 1,2-Dichloro-3-(2-methoxyethoxy)-4-methylsulfonylbenzene A solution of 10.0 g (35 mmol) of 1,2-dichloro-3-(2-methoxyethoxy)-4-methylsulfonylbenzene in 500 g of anhydrous dioxane was placed in a 1 L Hastalloy C pressure reactor equipped with a mechanical stirrer and was purged with nitrogen. The following were then added: 7.48 g (70 mmol) of 1-ethyl-5-hydroxypyrazole, 8.16 g (77 mmol of sodium carbonate, 0.195 g (1.75 mmol) of palladium acetate, 0.37 g (1.75 mmol) of 1,4-bisdiphenylphosphinobutane, 0.19 g (0.35 mmol) of hydroquinone, and 0.56 g (3.5 mmol) of tetrabutylammonium bromide. The reactor was sealed and purged three times with carbon monoxide, pressuring to about 200 psi (about 13,800 kiloPascals) each time and was then pressured to 150 psi (10,300 kiloPascals). The mixture was heated to 100-105¡ã C. with stirring, the pressure was adjusted to 175-200 psi (12,000 to 13,800 kiloPascals), and the reaction was allowed to proceed for about 50 hours. About 500 mL of water was added and the bulk of the dioxane was removed by evaporation under reduced pressure. The resulting mixture was filtered to remove spent catalyst, washed twice with 30 mL portions of toluene, and poured slowly with stirring into 200 mL of 10 percent aqueous hydrochloric acid, keeping the temperature at about 60¡ã C. The yellow solution obtained was allowed to cool and the precipitate that formed was collected by filtration, washed with water, and dried to obtain 9.0 g (59 percent of theory) of the title compound., 7688-25-7
The synthetic route of 7688-25-7 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Dow AgroSciences LLC; US6015911; (2000); A;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate