SCOPUS 정보 검색 플랫폼

Volumn 21, Issue 5, 2010, Pages 572-575

Synthesis of two new cage molecules containing trinitromethyl group

Author keywords

Cage compound; Synthesis; Trinitromethyl group; X ray crystal structure

Indexed keywords

EID: 77949915819 PISSN: 10018417 EISSN: None Source Type: Journal
DOI: 10.1016/j.cclet.2009.12.001 Document Type: Article

Times cited : (40)

References (14)

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13
- 77949916129
- At room temperature 10 mL acetic anhydride was dropped in 10 mL 98% nitric acid keeping the temperature below 30 °C. Then compound 2 (1.12 g, 2.96 mmol) was added into this mixture slowly. The reaction temperature was elevated to 50 °C. After 2 h the mixture was poured into ice-water. Compound 3 1.1 g (68.3, was obtained as white power and purified by recrystallization in acetone. After dissolving compound 3 (1.12 g, 2.5 mmol) in the mixture of 98% nitric acid (6 mL) and 25% Oleum(3 mL) at 0 °C, the reaction temperature was elevated to 80 °C and kept for 2 h .Then the reaction mixture was filtered and compound 4 0.6 g (52.6, was obtained, which was recrystallized from 67% nitric acid. The data of compound 3: FTIR IR (KBr, ν, cm-1, 3031, 1697, 1655, 1598, 1307; 1H NMR (400 MHz, CD3COCD3, δ 2.13-2.31 (m, 12H, 4CH3, 5.326 (s, 2H, CH2, 6.049-6.090 (d, 2H on C4 and C6, 6.808-6.739 t, 2H on C1
- -.

14
- 77949914451
- Crystal data of compound 3: empirical formula, C16H20N10O12·2CH3COCH3; molecular weight, 660.58; crystal dimensions, 0.50 mm × 0.40 mm × 0.40 mm; monoclinic; P21/n; a, 12.4121(15) Å, b, 16.309(2) Å, c, 14.4991(17) Å; β, 90.096(2, V, 2935.0(6) Å3; Z, 4; Dc, 1.495 Mg m-3; MoKa radiation cell parameters from 8194 reflections; θ, 3.06-27.50; μ, 0.126 mm-1; T, 93(2) K. Crystal data of compound 4: empirical formula, C8H8N14O16·2CH3COCH3; molecular weight, 672.44; crystal dimensions, 0.37 mm × 0.27 mm × 0.18 mm; triclinic; P-1; a, 8.008(3) Å, b, 11.839(4) Å, c, 14.309(5) Å; α, 94.427(3, β, 99.918(6, γ, 101.707(4, V, 1299.5(7) Å3; Z, 2; Dc, 1.718 Mg m-3; MoKa radiation cell parameters from 4418 reflection
- -1; T = 93(2) K. Crystallographic data for compound 3 and 4 have been deposited in the Cambridge Crystallographic Data Centre with the deposition numbers of CCDC 754913 and CCDC 754912. Copies of these data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336 033; or e-mail: deposit@ccdc.cam.ac.uk).

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