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ChemicalBook CAS DataBase List 2T2

2T2 synthesis

10synthesis methods
-

Yield:79135-69-6 87%

Reaction Conditions:

with copper(l) iodide;tetrakis(triphenylphosphine) palladium(0);water;sodium iodide at 20; for 5 h;

Steps:

(21) Diarylethynes 2a-r: General Procedure

General procedure: The appropriate aryldiazonium tetrafluoroborate 1 (0.4 mmol),CaC2 (77 mg, 1.2 mmol), Pd(PPh3)4 (23 mg, 0.02 mmol), CuI (8mg, 0.04 mmol), NaI (180 mg, 1.2 mmol), and H2O (173 mg, 9.6mmol) in DES (1:2 choline chloride-urea) (4 mL) were stirred atr.t. for 5 h. When the reaction was complete (TLC), H2O (2 mL)and EtOAc (2 mL) were added. The resulting mixture was subjectedto ultrasonication for 5 min, then filtered to removesolids. The liquor was extracted with EtOAc (3 × 10 mL), and theextracts were washed with saturated brine (3 × 10 mL). Theresulting organic phase was dried (Na2SO4) and concentratedunder reduced pressure. The residue was purified by columnchromatography (silica gel, PE-EtOAc).

References:

Ma, Xiaolong;Li, Zheng [Synlett,2021,vol. 32,# 6,p. 631 - 635] Location in patent:supporting information

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