PMDETA

AcronymDefinition
PMDETAN,n,n',n',n-Pentamethyldiethylenetriamine
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N,N,N', N',N"-pentamethyldiethylenetriamine (PMDETA, 99%; Acros), 2-bromoisobutyryl bromide (98%; Adamas), copper powder ([Cu.sup.0]), Cu[Br.sub.2], triethylamine (Shanghai Chemical), and 2-hydroxyethyl acrylate (98%; Adamas) were used as received.
PDMS-Br (0.8 g, 0.155 mmol), toluene (3 ml), CuCl (15.34 mg, 0.155 mmol), PMDETA (0.065 ml, 0.31 mmol), and a magnetic stir bar, were added to a three-necked flask.
Next, a solution of [CuCl.sub.2] (1.48 mg, 1.11 X [10.sup.-2] mmol) and PMDETA (2.34 [micro]L, 1.11 X [10.sup.-2] mmol) in anisole (1 mL) was added.
Sample EIM- Formulation (g) E ED43B ELVF MMT ESi[O.sub.2] ETi[O.sub.2] Voranol RN 490 100 100 100 100 100 100 DMCHA 1.6 1.6 2.0 1.6 2.0 2.0 PMDETA 0.6 0.6 0.6 0.6 0.8 0.8 B 8471 2.5 2.5 2.5 2.5 2.5 2.5 HFC 365 mfc 26.9 26.9 26.9 26.9 26.9 26.9 [H.sub.2]O 1.5 1.5 1.5 1.5 1.5 1.5 Voranate M 600 173.5 173.5 173.5 173.5 173.5 173.5 Dellite 43 B - 5 - - - - Dellite LVF - - 5 - - - IM-MMT - - - 5 - - Si[O.sub.2] - - - 5 - Ti[O.sub.2] 5 Density 32.2 34.7 32.7 36.6 32.0 34.1 [kg/[m.sup.3]] TABLE 2.
Foam Formulation (g) A B C D Voranol RN 490 100 100 100 100 Tegostab B8469 1.6 1.6 1.6 1.6 DMCHA 1.4 1.4 1.4 1.4 PMDETA 0.4 0.4 0.4 0.4 K15 0.2 0.2 0.2 0.2 [H.sub.2]O 1.5 1.5 1.5 1.5 HFC 245fa 19.29 19.29 19.29 19.29 Tedimon 385 159 159 159 151 density (kg/[m.sup.3]) 33.2 33.1 33.2 33.0 Table 2.
Copper[R] bromide (CuBr) (51 mg; 0.35 mmol), PMDETA (74.3 [micro]L; 0.36 mmol), BiBBr (52.2 [micro]L; 0.36 mmol), MPTMS (6 mL; 25.2 mmol), and 10 mL anisole were added to a round bottom flask.
0.02 mL solution of PMDETA (2 mmol) in 2.6 mL of THF was added into the round-bottom flask under a nitrogen atmosphere.
Potassium hydroxide, copper bromide, dimethyl-2,6-dibromoheptadioate (DM-2,6-DBHD), phenol, 1,1,2,2-tetrachloroethane, N,N,N,N,N-pentamethyldiethyltnaminc (PMDETA), triflouroacetic acid (TFA) was purchased from Aldrich chemical Co.
Poly(ethylene glycol) methyl ether acrylate (PEGMA, [M.sub.n] = 480g/mol, Aldrich) was passed through basic alumina column to remove the inhibitor Ethyl [alpha]-bromoisobutyrate (EBIB, 98%, Aldrich), 2,3,4,5,6-pentafluorobenzyl chloride (Aldrich 99%), CuCl ([greater than or equal to] 99.99%, Aldrich), CuBr (98%, Aldrich), sodium azide (Na[N.sub.3], Sigma-Aldrich), 2,2-bipyridine (bpy, 99%, Fluka), N, N, N', N", N" -pentamethyldiethylenetriamine (PMDETA, 99%, Aldrich), methanol ([greater than or equal to] 99.9, Aldrich), N, NThicyclohexylcarbodiimide (DCC, 99%, Aldrich), 4-(dimethylamino) pyridine (DMAP, [greater than or equal to] 99.99%, Aldrich), propiolic acid (99%, Aldrich), and N, N-dimethylformamide (DMF, 99%, Aldrich) were used as received.
Tetrahydrofuran (THF), 2-butanone (MEK), 1-propanol, methanol, ethanol (EtOH), acetonitrile (C[H.sub.3]CN), diethyl ether, deuterated solvents, benzophenone, MMA, 2-HEMA, allyl 2bromo-2-methylpropionate (ABIB), copper (I) bromide (CuBr), copper (I) chloride (CuCl), 2,2'-bipyridyl (Bpy), N,N,N',N',N"-pentamethyldiethylenetriamine (PMDETA), chromatographic stationary phases (neutral and basic aluminium oxide), phosphate buffer saline (PBS), BDP, and poly(2-hydroxyethyl methacrylate) (PHEMA, Mv ~ 20,000) were all purchased from Sigma-Aldrich.
The 2-MAdMA monomer and the N,N,N',N",N"-pentamethyldiethylenetriamine (PMDETA) ligand were dissolved in a toluene-DMF (7:3) mixed solvent in a two necked eggplant flask with constant stirring for 30 min at room temperature.