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CAS No. : | 12079-65-1 | MDL No. : | MFCD00001440 |
Formula : | C8H5MnO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 204.06 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P264-P270-P301+P310+P330-P405-P501 | UN#: | 2811 |
Hazard Statements: | H300 | Packing Group: | Ⅱ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61% | In tetrahydrofuran; for 23h;Irradiation; Inert atmosphere; | General procedure: A solution of [(C5H5)Mn(CO)3] (I) and a slight molar excessof the phosphane in tetrahydrofuran (THF, 120 ml) was irradiatedfor 7 h under argon. The colours of the solutionschanged from yellow to red with concomitant gas evolution.After further stirring for 16 h, the solvent was evacuated andthe residue dissolved in diethyl ether (Et2O) and filteredthrough a plug of silica gel. The solvent was evaporated againand the residue dissolved in the minimum amount of petroleumether. This solution was placed on top of a silica gelchromatography column (alumina in the case of 3a) and theproducts were eluted with a petroleum ether/Et2O (9:1 v/v)mixture. Evaporation of the eluate yielded the products asyellow powders. Recrystallization from petroleum ether (with some added Et2O) by slow evaporation in a refrigerator at5 C yielded crystals of all three compounds. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | In decalin; at 200℃; for 9h;Reflux; Inert atmosphere; | Under purified argon Mn2(CO)10 (980 mg, 2.51 mmol), dicyclopentadiene C10H12 (2.0 mL, 1960 mg, 14.9 mmol), and decaline (6 mL) were heated to reflux (oil bath temperature of ca. 200 C). A gas evolution started, which ceased after 6 h. After 9 h of heating, the reaction mixture was cooled to room temperature, filtered, and cooled to -20 C. Ayellow solid deposited, which was separated, washed with cold hexane, and dried in vacuo (yield: 600 mg, 59%). Cooling of the mother liquor to -78 C yielded an additional precipitate (yield: 350 mg, 34%). The crude product (950 mg, 93%) was sublimated in vacuo, which resulted in yellow crystals. Yield: 735 mg, 3.60 mmol, 72%. 1H NMR (CDCl3): δ = 4.76 (s,[40] Δν1/2 = 2Hz, 1JHC = 179 Hz) ppm. 13C NMR (CDCl3): δ = 224.8 (br., Δν1/2 = 50 Hz, CO), 82.7 (s, Δν1/2 = 5Hz, Cp) ppm. 55Mn NMR (CDCl3): δ = -2160 (br., Δν1/2 = 8.5 kHz) ppm. UV/Vis (hexane): λ (ε) = 216 (15000), 332 (1000) nm (Lmol-1cm-1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
for 0.25h;UV-irradiation; | 5.0mg <strong>[12079-65-1]CpMn(CO)3</strong> (0.024mmol) was dissolved in 2mL thf before it was subjected to 15min of UV laser photolysis (Brilliant B, 355nm, 20mJ/pulse, 10Hz) in an evacuated glass apparatus (25cm3 volume). The resultant CpMn(CO)2(thf) solution was then evacuated and frozen before 0.024mmol ligand L was added. The mixture was evacuated and left to mix at room temperature in the dark for 15min to afford orange CpMn(CO)2L. The CpMn(CO)2L solution was then studied using IR spectroscopy and ESI-MS spectrometry without further purification. | |
at 20℃; for 1h;Inert atmosphere; Schlenk technique; Irradiation; | All complexes were synthesised according to a similar methodologyas reported by Lugan [4]. <strong>[12079-65-1]CpMn(CO)3</strong> (0.612 g, 3.0 mmol)was dissolved in 40ml of dry THF and irradiated for 60 min at roomtemperature. Imidazol-2-ylidene L1 (0.714 g, 3.0 mmol) was addedto the reaction mixture via cannula and the reaction allowed to stirfor 90 min. The reaction colour turned to deep brown and themixture was subsequently filtered through a small aluminium oxidecolumn. The solvent was evaporated, the product redissolvedand purified with column chromatography with hexane:ethereluent to recover 1 as an orange oil. Yield (0.267 g (31%) %). | |
In neat (no solvent); at -40℃; for 1h;Inert atmosphere; UV-irradiation; | A yellow solution of <strong>[12079-65-1](η5-C5H5)Mn(CO)3</strong> (0.157 g, 0.770 mmol) in THF(30 mL) was UV-irradiated at -40 for 1 h. |
for 1h;UV-irradiation; Inert atmosphere; Schlenk technique; Glovebox; | A solution of [<strong>[12079-65-1]CpMn(CO)3</strong>] (56 mg, 0.27 mmol) is dissolved in 50 mL thf and irradiatedwith UV light for 1 h using a low-pressure mercury lamp (TQ 150). The pale-rose solutionis added to solid [Cp”2Zr(1:1-As4)] (1) (100 mg, 0.13 mmol). After stirring for 16 h atroom temperature, the solvent of the red-brown reaction mixture is removed in vacuo,extracted with 10 mL n-pentane and filtered via cannula. A red solution is obtained. Violetcrystals of 3 suitable for single crystal X-ray structure analysis were obtained by storing aconcentrated solution at 78 C. Crystalline yield: 15 mg (0.014 mmol, 11%).1H NMR (C6D6, 298 K): d [ppm] = 1.25 (s, 18 H, CCH3), 1.36 (s, 36 H, CCH3), 4.99 (t,2 H, C5H3tBu2), 5.26 (t, 2 H, C5H3tBu2), 5.42 (t, 2 H, C5H3tBu2); elemental analysis (%):calculated for [C40H52ZrAs4Mn2O4] (1097.62 gmol1): C, 43.77; H, 4.78; found: C, 42.68;H, 5.13; IR (toluene): [cm1] = 1928 (s), 1873 (s); LIFDI MS (toluene): m/z (%): 1095.9(M+, 42), 919.9 (M+-[CpMn(CO)2], 100); crystal data for C40H52As4Mn2O4Zr, triclinic, P 1P-1, a = 11.4684(3) Å, b = 12.1340(4) Å, c = 16.8248(4) Å, = 80.103(2), = 89.979(2), = 63.838(2), V = 2080.60(11) Å3. | |
at -40℃; for 0.833333h;UV-irradiation; Inert atmosphere; | A red solution obtained by theUV irradiation of C5H5Mn(CO)3 (0.06 g, 0.24 mmol)in THF (15 mL) at -40 for 50 min |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 51.8% 2: 29.8% | With tetrahydrofuran In tetrahydrofuran Irradiation (UV/VIS); Ar atmosphere; irradiation of CpMn(CO)3 (1000 W quartz-mercury lamp, 5°C, 3 h), addn. of Ph2PCCH, stirring (15°C, 2 h); solvent removal, chromy. (SiO2, petroleum ether/CH2Cl2 9:1, 4:1); elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
27% | In tetrahydrofuran; for 23h;Irradiation; Inert atmosphere; | General procedure: A solution of [(C5H5)Mn(CO)3] (I) and a slight molar excessof the phosphane in tetrahydrofuran (THF, 120 ml) was irradiatedfor 7 h under argon. The colours of the solutionschanged from yellow to red with concomitant gas evolution.After further stirring for 16 h, the solvent was evacuated andthe residue dissolved in diethyl ether (Et2O) and filteredthrough a plug of silica gel. The solvent was evaporated againand the residue dissolved in the minimum amount of petroleumether. This solution was placed on top of a silica gelchromatography column (alumina in the case of 3a) and theproducts were eluted with a petroleum ether/Et2O (9:1 v/v)mixture. Evaporation of the eluate yielded the products asyellow powders. Recrystallization from petroleum ether (with some added Et2O) by slow evaporation in a refrigerator at5 C yielded crystals of all three compounds. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94.5% | [0079] 5 g of cyclopentadienyl manganese tricarbonyl was weighed and dissolved in 60 mL anhydrous tetrahydrofuran. A solution of N-butyl lithium in hexane (19.1 mL, 1.6 mol/L) was dropwise added to the tetrahydrofuran solution under the protection of -78 C. argon. After the dropwise addition, 4.84 mL DMF was added to obtain a mixture which was stirred at room temperature for 2 h. After the reaction, 200 mL hydrochloric acid (3 N) was added to the resultant mixture, then 200 mL water was added, and the mixture obtained was extracted with hexane. The organic phase was washed with water and dried with anhydrous sodium sulfate, and after a process of reduced pressure distillation, 5.37 g brown solid (cyclopentadiene formaldehyde tricarbonyl manganese) was obtained with a yield of 94.5%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | A mixture of phthalic anhydride (5.92 g, 40 mmol) and aluminiumchloride (10.67 g, 80 mmol) in dichloromethane (80 ml)was stirred for 30 min on an ice bath. Then the solution ofC5H5Mn(CO)3 (8.12 g, 40 mmol) in CH2Cl2 (80 ml) was added dropwisefor 30 min and refluxed for 4 h. The resulting mixture waspoured into ice mixed with concentrated HCl (5 ml). After all icemelted, the pale-yellow precipitate (insoluble in water and CH2Cl2)was separated with Buchner funnel and purified by recrystallizationfrom boiling isopropyl alcohol.Yield: yellow crystal, 6.78 g, 51%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62.5% | [0073] 1 g of cyclopentadienyl manganese tricarbonyl was weighed and dissolved in 10 mL anhydrous tetrahydrofuran. A solution of N-butyl lithium in hexane (3.37 mL, 1.6 mol/L) was dropwise added to the tetrahydrofuran solution under the protection of -45 C. argon. After the dropwise addition, excess dry ice was added to obtain a mixture which was stirred at room temperature for 2 h. After the reaction, the solvent was evaporated under reduced pressure, and then water and ethyl acetate were added to the mixture obtained with being shaken greatly. Hydrochloric acid was added to |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With n-butyllithium; In tetrahydrofuran; hexane; at 20℃;Darkness; | Under purified argon nBuLi in hexane (2.5 m, 0.95 mL, 2.38 mmol) was diluted with hexane (4 mL) and added to a solution of <strong>[12079-65-1]CpMn(CO)3</strong> (408 mg,2.00 mmol) in THF (20 mL) cooled to -78 C with exclusion of light. After 1 h at -78 C, Et2NMe2SiCl (0.4 mL, 360 mg,2.17 mmol) in hexane (4.5 mL) was added slowly. After warming up to room temperature and stirring overnight, an orange-brown solution of Et2NMe2SiC5H4Mn(CO)3 was obtained |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In tetrahydrofuran; hexane; at -78℃; for 1h;Darkness; Inert atmosphere; | Under purified argon nBuLi in hexane (2.5 m, 0.95 mL, 2.38 mmol) was diluted with hexane (4 mL) and added to a solution of <strong>[12079-65-1]CpMn(CO)3</strong> (408 mg,2.00 mmol) in THF (20 mL) cooled to -78 C with exclusion of light. After 1 h at -78 C, Et2NMe2SiCl (0.4 mL, 360 mg,2.17 mmol) in hexane (4.5 mL) was added slowly. After warming up to room temperature and stirring overnight, an orange-brown solution of Et2NMe2SiC5H4Mn(CO)3 was obtained |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 100℃; for 168h; | Single crystals of the inclusion compound 1 wereobtained by keeping a mixture of crystals of the initial [Zn2(dmf)(bdc)(lac)]DMF with the excess of solid <strong>[12079-65-1]cymantrene</strong> ina closed evacuated glass tube at 100 for a week. The excess of <strong>[12079-65-1]cymantrene</strong> deposited in the upper part of the glass tube.When the tube was cooled and opened, crystals of the inclusion compound 1 were separated mechanically from the excess of <strong>[12079-65-1]cymantrene</strong>. |