CAS RN: 95464-05-4 | Product Number: B2064
[1,1'-Bis(diphenylphosphino)ferrocene]palladium(II) Dichloride Dichloromethane Adduct
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|Purity / Analysis Method||>98.0%(T)|
|Molecular Formula / Molecular Weight||C__3__4H__2__8Cl__2FeP__2Pd·CH__2Cl__2 = 816.64|
|Physical State (20 deg.C)||Solid|
|Packaging and Container||1G-Glass Bottle with Plastic Insert (View image)|
|PubChem Substance ID||87564938|
|Appearance||Light yellow to Amber to Dark green powder to crystal|
|Purity(Argentometric Titration)||min. 98.0 %|
|Melting Point||268 °C(dec.)|
|Hazard Statements||H302 + H312 + H332 : Harmful if swallowed, in contact with skin or if inhaled.
H315 : Causes skin irritation.
H319 : Causes serious eye irritation.
|Precautionary Statements||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/ protective clothing/ 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.
P332 + P313 : If skin irritation occurs: Get medical advice/ attention.
P362 : Take off contaminated clothing and wash before reuse.
P301 + P312 + P330 : IF SWALLOWED: Call a POISON CENTER/doctor if you feel unwell. Rinse mouth.
P302 + P352 + P312 : IF ON SKIN: Wash with plenty of water.Call a POISON CENTER/doctor if you feel unwell.
P304 + P340 + P312 : IF INHALED: Remove person to fresh air and keep comfortable for breathing. Call a POISON CENTER/doctor if you feel unwell.
To a solution of 2-bromo-3-methylpyridine (103 mg, 60 mmol) in degassed toluene (0.6 mL, 0.1 mol/L) and H2O (0.2 mL) was added 3-(tert-butoxycarbonyl)phenylboronic acid (150 mg, 0.66 mmol, 1.1 equiv), K2CO3 (398 mg, 2.9 mmol, 4.8 equiv), [1,1'-bis(diphenylphosphino)ferrocene]palladium(II) dichloride dichloromethane adduct (24.5 mg, 3.0 μmol, 5.0 mol%) and the mixture was stirred at reflux for 4 h. The reaction mixture was diluted with H2O (10 mL) and extracted with EtOAc (20 mL x 3). The solvent was removed under reduced pressure and the residue was purified by silica gel column chromatography (hexane : EtOAc = 1 : 0 to 4 : 1) to give 1 as a pale yellow oil (155 mg, 94%).
The reaction mixture was monitored by TLC (hexane : EtOAc = 2 : 1, Rf = 0.62).
Analytical Data（Compound 1）
1H NMR (400 MHz, CDCl3); δ 8.54 (brd, J = 5.0 Hz, 1H), 8.14 (q, J = 1.5 Hz, 1H), 8.03 (dt, J = 7.8, 1.4 Hz, 1H), 7.69 (dq, J = 7.6, 1.5 Hz, 1H), 7.60 (m, 1H), 7.51 (dt, J = 7.7, 1.1 Hz, 1H), 7.21 (dd, J = 7.8, 4.6 Hz, 1H), 2.36 (s, 3H), 1.58 (s, 9H).
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