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| Product Number | D6204 |
Purity / Analysis Method
|
>98.0%(T)(HPLC) |
| Molecular Formula / Molecular Weight | C__6H__1__5N·CH__2N__4 = 171.25 |
| Physical State (20 deg.C) | Solid |
Storage Temperature
|
Refrigerated (0-10°C) |
| Store Under Inert Gas | Store under inert gas |
| Condition to Avoid | Air Sensitive,Hygroscopic,Heat Sensitive |
| CAS RN | 93183-36-9 |
| Reaxys Registry Number | 3569216 |
| Appearance | White to Light yellow powder to crystal |
| Purity(HPLC) | min. 98.0 area% |
| Purity(Nonaqueous Titration) | min. 98.0 % |
| Melting point | 151.0 to 155.0 °C |
| NMR | confirm to structure |
| Melting Point | 152 °C |
| Pictogram |
|
| Signal Word | Warning |
| Hazard Statements | H315 : Causes skin irritation. H319 : Causes serious eye irritation. |
| Precautionary Statements | P264 : Wash skin thoroughly after handling. P280 : Wear protective gloves/ eye protection/ face protection. 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. P302 + P352 : IF ON SKIN: Wash with plenty of soap and water. P332 + P313 : If skin irritation occurs: Get medical advice/ attention. P362 : Take off contaminated clothing and wash before reuse. |
| HS Number | 2933.99.7900 |
2-Cyanoethyl N,N,N',N'-tetraisopropylphosphorodiamidite (0.7 mL, 2.2 mmol, 1.2 eq.) was added to a solution of DMT-T (1.0 g, 1.8 mmol) and diisopropylammonium tetrazole (160 mg, 0.92 mmol, 0.5 eq.) in dichloromethane (9.2 mL) at room temperature. After the completion of the reaction, saturated aq. NaHCO3 (5 mL) was added to the solution and extracted with dichloromethane (15 mL, twice). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (hexane:ethyl acetate = 70:30 - 50:50, 2% of triethylamine was added to the eluents) to give 1 (1.2 g, 88% yield) as a white crystal.
The reaction solution was monitored by NMR.
Compound 1
1H NMR (400 MHz, CDCl3); δ 11.36 (s, 1H), 7.50 (d, J = 4.0 Hz, 1H), 7.36-7.20 (m, 9H), 6.87-6.83 (m, 4H), 6.16-6.15 (m, 1H), 4.56-4.49 (m, 1H), 3.99 (d, J = 4.0 Hz, 1H), 3.73-3.72 (m, 1H), 3.22-3.19 (m, 1H), 2.72 (t, J = 8.0 Hz, 1H), 2.62 (t, J = 1.2 Hz, 1H), 2.41-2.31 (m, 1H), 1.44 (d, J = 1.2 Hz, 3H), 1.18-1.06 (m, 12H).
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