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85034475054
-
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note
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3 produced the less reactive dichloro product 3 in impure form.
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31
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0001391098
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-
36
-
-
85034471311
-
-
note
-
2, 3.5% EtOAc in hexanes, TMS compound elutes first) or more conveniently, by recrystallization from a minimal amount of hexanes at -4°C. The TMS bpy 1 precipitates and may be collected by filtration. The yellow impurity may be removed from the solid thus collected by washing with copious quantities of very cold hexanes, leaving the TMS product 1 as a white crystalline solid.
-
-
-
-
37
-
-
85034477506
-
-
note
-
3, followed by concentration of the organic layer.
-
-
-
-
39
-
-
85034459284
-
-
note
-
2Br: bp = 47°C), but also leads to side products and depressed yields in the alkylation reactions as compared with reactions run in DMF solution.
-
-
-
-
40
-
-
85034463505
-
-
note
-
Though the phenethyl product 7 is produced in good yield (83%, GC) by the CsF reaction, this drops dramatically during purification due to the difficulties of separation from the dimethyl bpy byproduct of similar polarity.
-
-
-
-
41
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0000324295
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43
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5244370033
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Timmers, F.J.5
-
44
-
-
85034469323
-
-
Rotoevaporation at elevated temperature results in decomposition of the "dry TBAF" reagent
-
Rotoevaporation at elevated temperature results in decomposition of the "dry TBAF" reagent.
-
-
-
-
45
-
-
84972811654
-
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Bos, K. D.; Kraaijkamp, J. G.; Noltes, J. G. Synth. Commun. 1979, 9(6), 497-504.
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Bos, K.D.1
Kraaijkamp, J.G.2
Noltes, J.G.3
-
46
-
-
85034479179
-
-
Melting points in ref 20a for mono- and dialkylated products appear to be transposed. The melting point reported for the monoalkyl bpy (76-77°C) is coincident with what we measured for the dialkylated product
-
Melting points in ref 20a for mono- and dialkylated products appear to be transposed. The melting point reported for the monoalkyl bpy (76-77°C) is coincident with what we measured for the dialkylated product.
-
-
-
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