CAS RN: 676525-77-2 | Product Number: D4887
|Size||Unit Price||Same Day||2-3 Business Days|
|Purity / Analysis Method||>85.0%(HPLC)|
|Molecular Formula / Molecular Weight||C__4__0H__4__0F__6IrN__4P = 913.97|
|Physical State (20 deg.C)||Solid|
|Condition to Avoid||Light Sensitive,Heat Sensitive|
|Reaxys Registry Number||17851176|
|PubChem Substance ID||253661441|
|Appearance||Light yellow to Yellow to Orange powder to crystal|
|Purity(HPLC)||min. 85.0 area%|
|Maximum Absorption Wavelength||380(CH2Cl2) nm|
|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.
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.
An oven-dried Schlenck tube was charged with N-(2-aminoethyl)-N-benzylglycine bis(trifluoroacetate) (88 mg, 0.20 mmol), and the system was degassed through N2 purging (3 x 5 min). 1 mol/L KOH solution in methanol (0.82 mL, 0.82 mmol) and 4-fluorobenzaldehyde (35 mg, 0.28 mmol) were subsequently added. The reaction mixture was stirred at room temperature for 0.5 h. A solution of [Ir(ppy)2(dtbbpy)]PF6 (1.8 mg, 2.0 x 10-3 mmol) in dry acetonitrile (3.2 mL) was added. The reaction was degassed with N2 bubbling before starting the irradiation and was stirred at room temperature under the exposure of blue LEDs for 3 h. The solution was filtered to remove the trifluoroacetate salt formed. The resulting mixture was concentrated under vacuum and purified with column chromatography (1 : 99 methanol / ethyl acetate on SiO2), giving 1-benzyl-3-(4-fluorophenyl)piperazine as a yellow oil (43 mg, 80%).
The reaction mixture was monitored by TLC (ethyl acetate, Rf = 0.25) and LCMS.
1H NMR (400 MHz, CDCl3); δ 7.35–7.20 (m, 7H), 6.99–6.91 (m, 2H), 4.29 (br, 1H) 3.94 (dd, 1H, J = 10.4, 2.8 Hz), 3.55 (s, 2H), 3.06–2.98 (m, 2H), 2.89–2.82 (m, 2H), 2.27 (ddd, 1H, 11.2, 9.2, 4.8 Hz), 2.20 (m, 1H).
13C NMR (101 MHz, CDCl3); δ 163.8, 161.3, 137.4, 135.7, 129.2, 128.4, 127.5, 115.5, 63.0, 59.5, 51.9, 45.5.
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