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ChemicalBook CAS DataBase List DTFS

DTFS synthesis

13synthesis methods
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Yield:90141-51-8 90%

Reaction Conditions:

with copper (I) iodide;1,10-Phenanthroline;hexamethyldisilathiane;potassium carbonate in 1-methyl-pyrrolidin-2-one at 120; for 14 h;Inert atmosphere;Sealed tube;

Steps:

4. General Procedure

General procedure: To a screw-capped test tube under a nitrogen atmosphere, 1.10-phenanthroline (0.05 mmol, 9.0 mg),iodobenzene 1 (1 mmol), potassium carbonate (1 mmol, 138.2 mg), CuI (0.05 mmol, 9.5 mg),N-methyl-2-pyrrolidone (1 mL), and 1,1,1,3,3,3-hexamethyldisilathiane (0.5 mmol, 89.2 mg) were added.After the tube was sealed with a cap, the mixture was heated at 120 °C for 14 h. After the reaction, H2O wasadded to the mixture, which was then extracted with EtOAc three times. The combined organic phases wereevaporated under reduced pressure. The crude material was purified by silica gel column chromatography togive the corresponding diaryl sulfide 2.

References:

Ogiwara, Yohei;Maeda, Hiromu;Sakai, Norio [Synlett,2018,vol. 29,# 5,art. no. SS-2017-U0702-L,p. 655 - 657] Location in patent:supporting information