Maximum quantity allowed is 999
CAS RN: 14338-32-0 | 產品號碼: C0903
2-Chloro-1-methylpyridinium Iodide
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產品號碼 | C0903 |
純度/分析方法 | >98.0%(T) |
分子式 / 分子量 | C__6H__7ClIN = 255.48 |
外觀與形狀(20°C) | Solid |
儲存條件 | Room Temperature (Recommended in a cool and dark place, <15°C) |
儲存在惰性氣體下 | Store under inert gas |
應避免的情況 | Light Sensitive,Hygroscopic |
CAS RN | 14338-32-0 |
Reaxys-RN | 3572320 |
PubChem Substance ID | 87565959 |
SDBS (AIST Spectral DB) | 10163 |
Merck Index(14) | 6301 |
MDL編號 | MFCD00011984 |
Appearance | Light yellow to Amber to Dark green powder to crystal |
Purity(HPLC) | min. 95.0 area% |
Purity(Nonaqueous Titration) | min. 98.0 % |
Solubility in Water | almost transparency |
圖形表示 |
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信號詞 | Warning |
危險性說明 | H315 : Causes skin irritation. H319 : Causes serious eye irritation. |
防範說明 | P264 : Wash skin thoroughly after handling. P280 : Wear protective gloves/ eye protection/ face protection. P302 + P352 : IF ON SKIN: Wash with plenty of water. 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. |
HS編碼* | 2933.39-000 |
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Used Chemicals
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Procedure
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Boc-Pro-OH (1.65 g, 7.65 mmol), 2-chloro-1-methylpyridinium iodide (1.95 g, 7.65 mmol) were added to solution of H-Phe-OMe・HCl (1.50 g,6.95 mmol) in dichloromethane (30 mL) at room temperature and triethylamine (3.40 mL, 24.3 mmol) was added dropwise in 3 min at 5 to 10 °C. After stirring for 3 h, solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate and washed with 10% citric acid aq. (30 mL × 3), 5% sodium bicarbonate solution aq. (30 mL × 3) and brine (30 mL). The organic layer was dried over anhydrous sodium sulfate and filtered. After the removal of solvent under reduced pressure, the given crude was purified by column chromatography (hexane : EtOAc = 2 : 1) to give Boc-Pro-Phe-OMe (2.37 g,91%) as a slightly yellowish solid.
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Experimenter's Comments
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Consumption of stating material and formation of product was monitored by LCMS.
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Analytical Data(Boc-Pro-Phe-OMe)
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1H NMR (400 MHz, DMSO-d6); δ 8.17–8.27 (m, 1H), 7.19–7.29 (m, 5H), 4.42–4.53 (m, 1H), 4.00–4.13 (m, 1H), 3.56–3.61 (m, 3H), 3.18–3.38 (m, 2H), 2.90–3.08 (m, 2H), 1.91–2.11 (m, 1H), 1.56–1.71 (m, 3H), 1.15-1.40 (m, 9H).
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Lead Reference
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- A facile synthesis of carboxamides by using 1-methyl-2-halopyridinium iodides as coupling reagents
References
- 1) A CONVENIENT METHOD FOR THE SYNTHESIS OF CARBOXYLIC ESTERS
- 2) A FACILE SYNTHESIS OF CARBOXAMIDES BY USING 1-METHYL-2-HALOPYRIDINIUM IODIDES AS COUPLING REAGENTS
- 3) Asymmetric Decarboxylative Allylation of Oxindoles
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