Tetrahydrofuran → HCID 59806151, Verbindung

Firstly, a mixture of 4,4′-diiodotolan (171 mg, 0.40 mmol), PdCl2(PPh3)2 (27.9 mg, 0.040 mmol) and CuI (7.6 mg, 0.040 mmol) was added with dist. THF (3 mL), dist. Et3N (3 mL) and trimethylsilylacetylene (140 μL, 0.99 mmol). The resultant mixture was then stirred under a nitrogen atmosphere at 50° C. for 17 hours to obtain a reaction mixture. Subsequently, the reaction mixture was diluted with CH2Cl2. After that, an organic layer was washed with sat. NaCl, and the washed organic layer was then dried with MgSO4. The dried organic layer was filtered and concentrated to obtain a crude product (I). The obtained crude product (I) was separated and purified by silica gel column chromatography (hexane/EtOAc=10/1) to obtain 4,4′-bis(trimethylsilylethynyl)tolan.

1. additionwas added with dist
2. customto obtain a reaction mixture
3. washAfter that, an organic layer was washed with sat. NaCl
4. dry with materialthe washed organic layer was then dried with MgSO4
5. filtrationThe dried organic layer was filtered
6. concentrationconcentrated
7. customto obtain a crude product (I)
8. customThe obtained crude product (I)
9. customwas separated
10. custompurified by silica gel column chromatography (hexane/EtOAc=10/1)

ORD-Eintrag

ord-315e6b72c12c4ae9b03e85e5115c85fc

Quelldatensatz

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08053588B2