Maximum quantity allowed is 999
CAS RN: 19172-47-5 | 產品號碼: B1133
Lawesson's Reagent [Sulfurating Reagent]
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產品號碼 | B1133 |
純度/分析方法 | >93.0%(T) |
分子式 / 分子量 | C__1__4H__1__4O__2P__2S__4 = 404.45 |
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 | Moisture Sensitive |
CAS RN | 19172-47-5 |
Reaxys-RN | 1024888 |
PubChem Substance ID | 87564076 |
Merck Index(14) | 5391 |
MDL編號 | MFCD00005171 |
Appearance | White to Light yellow to Green powder to crystal |
Purity(Iodometric Titration) | min. 93.0 % |
熔點 | 230 °C |
圖形表示 | |
信號詞 | Warning |
危險性說明 | H302 + H332 : Harmful if swallowed or if inhaled. H315 : Causes skin irritation. H319 : Causes serious eye irritation. |
防範說明 | P501 : Dispose of contents/ container to an approved waste disposal plant. P261 : Avoid breathing dust/ fume/ gas/ mist/ vapors/ spray. P270 : Do not eat, drink or smoke when using this product. P271 : Use only outdoors or in a well-ventilated area. 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. P301 + P312 + P330 : IF SWALLOWED: Call a POISON CENTER/doctor if you feel unwell. Rinse mouth. P304 + P340 + P312 : IF INHALED: Remove person to fresh air and keep comfortable for breathing. Call a POISON CENTER/doctor if you feel unwell. |
HS編碼* | 2931.49-900 |
Used Chemicals
Procedure
To a solution of Lawesson’s reagent (2.38 g, 5.88 mmol) in dichloromethane (42 mL), 2-pyrrolidone (1.0 g, 11.75 mmol) in dichloromethane (42 mL) was added at room temperature under N2 atmosphere. After stirring the reaction solution for 2 hours, the solvent was removed under reduced pressure and the residue was purified by column chromatography (hexane:ethyl acetate = 9:1 - 6:4), giving pyrrolidine-2-thione as a white solid (0.79 g, 66%).
Experimenter’s Comments
The reaction was carried out in the fume hood due to Lawesson’s reagent’s bad smell.
The reaction mixture was monitored by TLC (hexane:ethyl acetate = 3:2, Rf = 0.28).
Analytical Data(pyrrolidine-2-thione)
1H NMR (400 MHz, CDCl3); δ 8.61 (brs, 1H), 3.61 (t, 2H, J = 8.0 Hz), 2.86 (t, 2H, J = 8.0 Hz), 2.20-2.12 (m, 2H).
13C NMR (101 MHz, CDCl3); δ 205.83, 49.66, 43.21, 22.91.
Lead Reference
- Ruthenium Catalyzed Synthesis of Enaminones
References
- S. O. Lawesson, et al., Bull. Soc. Chim. Belg. 1978, 87, 223; 87, 229; 87, 293; 87, 299.
- R. Shabana, et al., Nouv. J. Chim. 1980, 4, 47.
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