Electrochemical Synthesis of Pd Nanoparticles on Pencil-Graphite and Application for Suzuki

Supplementary Information for

Electrochemical synthesis of Pd nanoparticles on Pencil-Graphite and application for Suzuki coupling reactions.

Kishor E. Balsane, Radheshyam S. Shelkar, and Jayashree M. Nagarkar*

Department of Chemistry, Institute of Chemical Technology, Matunga, Mumbai – 400019, India.

*Corresponding author. Tel.: +91 22 33611111/2222; fax: +91 22 33611020.

Email: ;

S1. Preparation of PdNP-PGcatalyst:

In the synthesis of PdNP-PG,conventional three electrode cyclic voltammetry potentiostat / galvanostat (PGSTAT302N) equipped with GPES software was used for electrodeposition on PG.

Figure 1:The electrodeposition carried out at -0.2V at 25 °C for 10 second

Figure 2: The electrodeposition curve at -0.2V at 25 °C for 10 second.

Figure 3: The Electron diffraction image of PdNP-PG.

Figure 4 :EDX image of PdNP-PG.

Figyre: 5TGA image of PdNP-PG

Figure 6: Scraped catalyst PdNP-PG.

Figure 7:Dispersion PdNP-PGin water (a), settled catalyst (b)

S2.Spectral data of selected compound of Suzuki reaction:

1) 1,1'-biphenyl (table 2 entry 1)

GC-MS DATA-

MS (m/z/rel.int.): 154(M+): 51(8.1), 76(26.5), 154(100).

1HNMR

1H NMR (300 MHz, CDCl3): δ =7.21-7.30(m, 2H), 7.32-7.40(m, 4H), 7.54-7.59(m, 4H).

2) 4-methyl-1,1'-biphenyl (table 2 entry 2).

GC-MS DATA-

MS (m/z/rel.int.): 168(M+): 51(4.1), 83(9.8), 152(23.6), 168(100).

3) 4-methoxy-1,1'-biphenyl (table 2 entry 3)

GC-MS DATA-

MS (m/z/rel.int.): 184(M+): 51(4.0), 76(7.5), 115(33.7), 141(47.9),169(53.5), 184(100).

1HNMR-

1H NMR (300 MHz, CDCl3): δ =3.85(s, 3H), 7.1(d, 2H),7.21(d,1H),7.32(d,2H),7.43(t,2H),7.54(t,2H).

4) 1-([1,1'-biphenyl]-4-yl)ethanone (Table 2, entry 4).

GC-MS DATA-

MS (m/z/rel.int.): 196(M+): 43(11.6), 76(20.3), 152(58.2), 181(100),196 (52.7).

1HNMR-

1H NMR (300 MHz, CDCl3): δ =2.62(s,3H),7.38-7.51(m,3H),7.63-7.73(m,4H),8.07(d,2H).

5) 1,1'-biphenyl]-4-ol(Table 2, entry 5).

GCMS DATA:

MS (m/z/rel.int.): 170(M+): 51(3.8), 115(17.9), 141(25.9), 170(100).

H1 NMR

1H NMR (300 MHz, CDCl3): δ =5.0(s, 1H), 6.95 (d, 1H), 7.30(s, 1H), 7.40-7.73(m, 6H), 8.34(d, 1H).

6) 4-nitro-1,1'-biphenyl (table 2ntry 6).

GC-MS DATA-

MS (m/z/rel.int.): 199(M+): 51(12.0), 76(17.9), 152(99.5), 169(36.7),199 (100).

7) 4-fluoro-1,1'-biphenyl(Table 2, entry 7).

MS (m/z/rel.int.): 172(M+): 51(4.0), 76(5.4), 85(10.6), 152(4.6),172(100).

8) 1,1'-biphenyl]-4-carbonitrile(Table 2, entry 8).

MS (m/z/rel.int.): 179(M+): 51(5.3), 76(12.6), 151(16.7), 179(100).

9) 2-methyl-1,1'-biphenyl(Table 2, entry 10).

MS (m/z/rel.int.): 168(M+): 51(6.8), 83(17.5), 153(49.1), 167(92.3),168(100).

10) 3-fluoro-1,1'-biphenyl(Table 2, entry 11).

MS (m/z/rel.int.): 172(M+): 51(4.5), 85(10.1), 172(100).

11) 3,5-dimethyl-1,1'-biphenyl(Table 2, entry 12).

MS (m/z/rel.int.): 182(M+): 51(5.1), 76(7.9), 152(16.1), 167(59.2), 182(100).

12) 2-phenylthiophene(Table 2, entry 14).

MS (m/z/rel.int.): 160(M+): 51(5.9), 115(39.5), 128(14.9), 160(100).

13) 2-phenylpyridine(Table 2, entry 15).

MS (m/z/rel.int.): 155(M+): 51(16.8), 77(20.8), 127(19.0), 155(100).

14) 4-chloro-1,1'-biphenyl(Table 2, entry 16).

MS (m/z/rel.int.): 188(M+): 51(27.6),63(19.5), 76(29.9), 152(74.7), 188(100).

15) 4-chloro-4'-methyl-1,1'-biphenyl(Table 2, entry 17).

MS (m/z/rel.int.): 202(M+): 82(24.7), 152(22.4), 167(58.7), 202(100).

16) 4-chloro-4'-methoxy-1,1'-biphenyl(Table 2, entry 18).

MS (m/z/rel.int.): 218(M+): 63(2.3),76(1.7), 109(5.2), 139(22.9), 149(10.7), 175(36.1), 203(7.2), 218(100).

17) 1-(4'-chloro-[1,1'-biphenyl]-4-yl)ethanone(Table 2, entry 19).

MS (m/z/rel.int.): 230(M+): 43(21.2), 76(23.2), 152(77.2), 215(100), 230(45.6).

18) 4-chloro-4'-nitro-1,1'-biphenyl(Table 2, entry 20).

MS (m/z/rel.int.): 233(M+): 51(6.2), 63(8.4), 76(6.0), 125(4.5), 152(100), 175(19.0), 203(31.5), 233(94.0).

19)2-chloro-1,1'-biphenyl(Table 2, entry 21).

MS (m/z/rel.int.): 188(M+): 51(27.6), 63(19.5), 76(29.9), 152(74.7), 188(100).