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Organometallics
Volumn 26, Issue 5, 2007, Pages 1126-1128
Sugar-incorporated N-heterocyclic carbene complexes
Author keywords

[No Author keywords available]
Indexed keywords

ALCOHOLS; IRIDIUM; SYNTHESIS (CHEMICAL); X RAY CRYSTALLOGRAPHY;
EID: 33947241996     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om061128d     Document Type: Article
Times cited : (59)
References (47)
  • 41
    • 33947195592 scopus 로고    scopus 로고
    • Synthesis of 2: Ag2O (23 mg, 0.10 mmol) was added to a solution of 1HBr (100 mg. 0.20 mmol) in DMSO (2 mL, After it was stirred for 4 h, the mixture was filtered through Celite. The filtrate was poured into water to afford a white precipitate of the complex, which was collected by filtration and dried under vacuum. Because the complex slowly decomposed during purification, satisfactory elemental analysis data could not be obtained. 1H NMR (400 MHz. DMSO-d6, δ 7.74 (d. 2H, 4-imidazolylidene, 7.50 (d, 2H, 5-imidazolylidene, 6.10 (d. 2H, 1-glucose, 5.55 (t, 2H, 3-glucose, 5.48 (t, 2H, 2-glucose, 5.22 (t. 2H. 4-glucose, 4.37 (m, 2H, 5-glucose, 4.32 (d. 4H. 6-glucose, 3.82 (s. 6H, CH, N, 2.04 (s, 6H, CH3 AcO, 2.02 (s, 6H, CH3 AcO, 1.98 (s, 6H, CH 3 AcO, 1.88 (s, 6H, CH3, AcO, 13C NMR (400 MHz, DMSO-d6, δ 180.86 (2-imidazolylidene, 170.5 (C=O, 170.0 (C=O, 169.9 C
    • +).
  • 42
    • 33947272849 scopus 로고    scopus 로고
    • 2O (116 mg. 0.50 mmol) was added to a solution of 1HBr ( 100 mg, 0.20 mmol) in acetone (2 mL). After it was stirred for 2 h, the mixture was filtered through Celite to give a pale yellow filtrate, which was dried under reduced pressure to afford a light yellow material.
    • 3 AcO).
  • 44
    • 33947208733 scopus 로고    scopus 로고
    • Synthesis of 4. Method A: Ag2O (23 mg, 0.10 mmol) was added to a solution of 1HBr (98 mg, 0.20 mmol) in acetone (2 mL, and the mixture was stirred at room temperature for 1 h. After removal of the insoluble solids by filtration using Celite, the solvent was removed under reduced pressure to give 3. A solution of [IrCp*Cl2]2 (80 mg, 0.10 mmol) in CH4Cl2 (5 mL) was added to 3. After the mixture was stirred for 18 h, insoluble solids were filtered off to give a yellow filtrate, from which the solvent was removed under reduced pressure to afford yellow microcrystals of 4 (yield: 45 mg, 0.055 mmol, 55, Method B: Ag4 (58 mg, 0.25 mmol) was added to a solution of 1HBr (250 mg, 0.51 mmol) in CH 4Cl2 (5 mL, After the mixture was stirred for 1 h at room temperature, IrCp*Cl2]2 (200 mg, 0.25 mmol) was added to the reaction mixture and the mixture was stirred for a further
    • +).
  • 46
    • 33947282993 scopus 로고    scopus 로고
    • Crystal data for 4: C28H39Cl2IrN 2O9, Mr, 810.75, size 0.20 × 0.05 × 0.05 mm, monoclinic, space group P21. a, 13.962(3) Å, b, 14.058(2) Å, c, 17.559(3) Å, β, 98.762(4)°, F(000, 1616, V, 3406.3(10) Å3. T= 193(1) K, Z, 4, Dcaled, 1.581 Mg/m3, μ, 4.1364 mm-1, refinement method full-matrix least squares on F2, R1, 0.0557 (observed data with I > 2σ(I, wR2, 0.0934, GOF, 1.021, Flack parameter 0.0167
    • 2, R1 = 0.0557 (observed data with I > 2σ(I), wR2 = 0.0934, GOF = 1.021, Flack parameter 0.016(7).

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.