Tetrahydrofuran → 1,4-Diethynylbenzene

참여 물질

역할	이름	HCID	투입량
반응물	Tetrahydrofuran	HCID 8028	—
반응물	Triethylamine	HCID 8471	—
반응물	p-Diiodobenzene	HCID 12208	—
반응물	Trimethylsilylacetylene	HCID 66111	—
촉매	Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)	HCID 24350	—
촉매	HCID 178418476	HCID 178418476	—
용매	Dichloromethane	HCID 6344	—
생성물	1,4-Diethynylbenzene	HCID 120463	—

반응 단계

Firstly, a mixture of 1,4-diiodobenzene (4 g, 12.1 mmol), PdCl2(PPh3)2 (340 mg, 0.484 mmol) and CuI (92.4 mg, 0.484 mmol), was added with dist. THF (20 mL), dist. Et3N (60 mL) and trimethylsilylacetylene (3.77 mL, 26.7 mmol). The resultant mixture was stirred under a nitrogen atmosphere at 80° C. for 22 hours to obtain a reaction mixture. Then, the reaction mixture was diluted with CH2Cl2. After that, an organic layer was washed with sat. NaCl, and dried with MgSO4. The dried organic layer was filtered and concentrated to obtain a crude product. The obtained crude product was separated and purified by silica gel column chromatography (hexane/EtOAc=10/1) to obtain 1,4-diethynylbenzene.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08053588B2
출처 데이터셋	uspto-grants-2011_11
ORD ID	ord-6034d2caa9fe431b851a0cf58f3e4f58
출처 메모	uspto-grants-2011_11