SCOPUS 정보 검색 플랫폼

Volumn , Issue 2, 2009, Pages 257-259

Formation of polysubstituted tetrahydrofurans on an iron tricarbonyl η5-pentadienyl template

Author keywords

Cycloaddition; Diene complexes; Iron

Indexed keywords

EID: 62349106059 PISSN: 09365214 EISSN: 14372096 Source Type: Journal
DOI: 10.1055/s-0028-1087516 Document Type: Article

Times cited : (18)

References (19)

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13
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- Typical Procedure, Preparation of Complex 4e Iron tricarbonyl 2-buta-1,3-dienyl-cyclopropane-1,1-dicarboxylic acid dimethyl ester (0.100 g, 0.29 mmol) was added to a flame-dried round-bottom flask under an atmosphere of nitrogen and dissolved in dry CH2Cl2 (5 mL, p-Anisaldehyde (0.060 g, 0.60 mmol) and ZnBr2 (0.193 g, 0.86 mmol) were added and the reaction mixture stirred for 1.0 h at r.t. The resulting mixture was filtered through a pad of Celite and SiO2, then concentrated in vacuo, and the residue purified by silica flash chromatography eluting in PE-Et2O (4:1 v/v) to yield the two inseparable title complex diastereomers as a yellow-orange oil (0.101 g, 73, dr, 4:1, HRMS-FAB: m/z calcd for C22H22O9Fe, M, 486.0613; found: 486.0623. IR (neat film, νmax, 3006, 2954, 2841 (sp3 CH, 2048, 1979 (MCO, 1742, 1738, 1732 (C=O) cm1
- +], 430 (28), 402 (66), 135 (100).

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15
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- Crystal Data for 4a C18H20FeO10, M, 452.19, a, 7.4917 (12, b, 10.4811 (16, c, 13.916 (2) Å, a, 72.126 (3, b, 78.035 (3, g, 74.455 (2)°, V, 992.6 (3) Å3; colourless crystal, 0.76 x 0.04 x 0.02 mm3, Dcalc, 1.513 g cm -3, m, 0.813 mm1, 7243 data, 3482 unique (Rint, 0.0381, Data were measured on a Bruker SMART 1000 diffractometer with MoKα radiation at 150 K. Data were corrected for absorption. The structure was solved by Patterson synthesis and refined on F2 values; H atom coordinates on atoms C(6, C(7, C(8, and C(9) were freely refined, other H atom parameters were constrained; R, 0.0432 [for 2567 observed data with F2 > 2σ(F2, and wR, 0.1046 for all data, Deposition no. 696186
- 2)] and wR = 0.1046 (for all data). Deposition no. 696186. Crystal data have been deposited with the Cambridge Crystallographic Data Centre. Data can be retrieved in CIF format by quoting the relevant deposition number in an e-mail request to deposit@ccdc.cam.ac.uk.

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