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CAS RN: 87413-09-0 | 产品编码: D2045
Dess-Martin Periodinane

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本品在储存过程中会产生一些不溶物。对反应性没有影响,请根据需要过滤后使用。
产品编码 | D2045 |
纯度/分析方法 | >95.0%(T) |
分子式/分子量 | C__1__3H__1__3IO__8 = 424.14 |
外观与形状(20°C) | 固体 |
储存温度 | 冷冻 (-20°C) |
储存在惰性气体下 | 存放于惰性气体之中 |
应避免的情况 | 光,空气,湿气 (分解),加热 |
包装和容器 | 1G-Glass Bottle with Plastic Insert (查看图片) |
CAS RN | 87413-09-0 |
Reaxys-RN | 4548207 |
PubChem物质ID | 87568496 |
Merck Index (14) | 2933 |
MDL编号 | MFCD00130127 |
Appearance | White to Almost white powder to crystal |
Purity(Iodometric Titration) | min. 95.0 % |
NMR | confirm to structure |
熔点 | 124 °C(dec.) |
溶解性(可溶于) | 氯仿, 丙酮 |
溶解性(微溶于) | 乙醚 |
象形图 |
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信号词 | Warning |
危险性说明 | H315 : Causes skin irritation. H319 : Causes serious eye irritation. H341 : Suspected of causing genetic defects. H272 : May intensify fire; oxidizer. |
防范说明 | P501 : Dispose of contents/ container to an approved waste disposal plant. P202 : Do not handle until all safety precautions have been read and understood. P220 : Keep/Store away from clothing/ combustible materials. P210 : Keep away from heat. P201 : Obtain special instructions before use. P221 : Take any precaution to avoid mixing with combustibles. P264 : Wash skin thoroughly after handling. P280 : Wear protective gloves/ protective clothing/ eye protection/ face protection. P302 + P352 : IF ON SKIN: Wash with plenty of water. P370 + P378 : In case of fire: Use dry sand, dry chemical or alcohol-resistant foam to extinguish. P308 + P313 : IF exposed or concerned: Get medical advice/ attention. P337 + P313 : If eye irritation persists: Get medical advice/ attention. P305 + P351 + P338 : IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. P362 + P364 : Take off contaminated clothing and wash it before reuse. P332 + P313 : If skin irritation occurs: Get medical advice/ attention. P405 : Store locked up. |
UN编号 | UN1479 |
类别 | 5.1 |
包装类别 | III |
HS编码* | 2934.99-000 |
Used Chemicals
Procedure
To dichloromethane (10 mL) was added trans-2-phenyl-1-cyclohexanol (0.30 g,1.7 mmol) and DMP (0.72 g, 1.7 mmol) at room temperature. The reaction mixture was stirred overnight at room temperature, then diluted with diethyl ether and washed with saturated aqueous sodium bicarbonate, 10% aqueous sodium thiosulfate, water and brine. The organic layer was concentrated under reduced pressure. The resulting crude product was purified by column chromatography (hexane:ethyl acetate = 8:1 on silica gel) to give 1 as a white solid (0.22 g, 74% yield).
Experimenter’s Comments
The reaction mixtures were monitored by TLC (hexane:ethyl acetate = 4:1).
Analytical Data(2-Phenylcyclohexanone (1))
1H NMR (400 MHz, CDCl3); δ 7.37-7.31 (m, 2H), 7.30-7.22 (m, 1H), 7.17-7.12 (m, 2H), 3.62 (dd, 1H, J = 12.4, 6.9 Hz), 2.58-2.41 (m, 2H), 2.33-2.23 (m, 1H), 2.22-2.10 (m, 1H), 2.10-1.94 (m, 2H), 1.91-1.75 (m, 2H).
13C NMR (101 MHz, CDCl3); δ 210.5, 138.9, 128.6, 128.5, 127.0, 57.5, 42.3, 35.2, 27.9, 25.5.
Lead Reference
- Acceleration of the Dess-Martin Oxidation by Water
References
- M. Horikawa, K. Hashimoto, H. Shirahama, Tetrahedron Lett. 1993, 34, 331.
- J. N. Haseltine, M. P. Cabal, N. B. Mantlo, N. Iwasawa, D. S. Yamashita, R. S. Coleman, S. J. Danishefsky, G. K. Schulte, J. Am. Chem. Soc. 1991, 113, 3850.
- J. P. Burkhart, N. P. Peet, P. Bey, Tetrahedron Lett. 1988, 29, 3433.
- D. B. Dess, J. C. Martin, J. Org. Chem. 1983, 48, 4155.
- R. J. Linderman, D. M. Graves, Tetrahedron Lett. 1987, 28, 4259.
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