Published TCIMAIL newest issue No.199
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| Product Number | A1246 |
| Molecular Formula / Molecular Weight | C__8H__1__4N__2O__4 = 202.21 |
| Physical State (20 deg.C) | Liquid |
Storage Temperature
|
Refrigerated (0-10°C) |
| Condition to Avoid | Light Sensitive,Heat Sensitive |
| CAS RN | 2446-83-5 |
| Reaxys Registry Number | 5262252 |
| MDL Number | MFCD00008875 |
| Appearance | Light yellow to Amber to Dark green clear liquid |
| Concentration(Iodometric titration) | 40.0 to 44.0 w/w% |
| NMR | confirm to structure |
| Specific Gravity (20/20) | 0.94 |
| Refractive Index | 1.47 |
| Pictogram |
|
| Signal Word | Danger |
| Hazard Statements | H312 + H332 : Harmful in contact with skin or if inhaled. H315 : Causes skin irritation. H319 : Causes serious eye irritation. H370 : Causes damage to organs. H372 : Causes damage to organs through prolonged or repeated exposure. H335 : May cause respiratory irritation. H361d : Suspected of damaging the unborn child. H336 : May cause drowsiness or dizziness. H304 : May be fatal if swallowed and enters airways. H225 : Highly flammable liquid and vapour. |
| Precautionary Statements | P260 : Do not breathe dust/ fume/ gas/ mist/ vapours/ spray. P210 : Keep away from heat, hot surfaces, sparks, open flames and other ignition sources. No smoking. P201 : Obtain special instructions before use. P280 : Wear protective gloves/ protective clothing/ eye protection/ face protection. P370 + P378 : In case of fire: Use dry sand, dry chemical or alcohol-resistant foam to extinguish. P331 : Do NOT induce vomiting. P308 + P311 : IF exposed or concerned: Call a POISON CENTER/doctor. P301 + P310 : IF SWALLOWED: Immediately call a POISON CENTER/doctor. |
| EC Number | 219-502-8 |
| UN Number | UN1993 |
| Class | 3 |
| Packing Group | II |
| HS Number | 2927000090 |
To a solution of triphenylphosphine (0.88 g, 3.4 mmol), 5-mercapto-1-phenyl-1H-tetrazole (0.79 g 4.4 mmol), 3-phenylpropan-1-ol (0.30 g, 2.2 mmol) in anhydrous tetrahydrofuran (22 mL) was added DIAD (40% in toluene, 2.1 mL, 4.0 mmol) at 0 °C and the mixture was stirred at rt for 1 hour. The solution was dropped into water (40 mL). The mixture was extracted with ethyl acetate (40 mL x 3), and organic phase was dried over sodium sulfate and filtered. The solvent was removed under reduced pressure and the residue was purified by column chromatography (ethyl acetate:hexane = 1:9 on silica gel) to give 1 (0.68 g, quant) as a white solid.
The reaction mixture was monitored by TLC (ethyl acetate:hexane = 1:9, Rf = 0.29).
Compound 1
1H NMR (400 MHz, CDCl3); δ 7.63-7.50 (m, 5H), 7.35-7.26 (m, 2H), 7.23-7.14 (m, 3H), 3.40 (t, J = 7.0 Hz, 2H), 2.79 (t, J = 7.6 Hz, 2H), 2.18 (quin, J = 7.3 Hz, 2H)
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