有沒(méi)有大佬

大佬們幫幫忙

首先你的原料也測(cè)試核磁了嗎？這個(gè)反應(yīng)容易出現(xiàn)2溴代物 TLC分點(diǎn)開(kāi)的話 柱層析應(yīng)該也能分開(kāi)

2溴代55%收率
Benzylic brominations with N-bromosuccinimide in (trifluoromethyl)benzene
By Suarez, Diana et al
From Synthesis, (11), 1807-1810; 2009

1溴代
Reactions of 2,6-di-tert-butylpyridine derivatives with methyl fluorosulfonate under high pressure

By Hou, C. J. and Okamoto, Yoshiyuki
From Journal of Organic Chemistry, 47(10), 1977-9; 1982


Benzylic brominations with N-bromosuccinimide in (trifluoromethyl)benzene

By Suarez, Diana et al
From Synthesis, (11), 1807-1810; 2009



Synthesis of Some Fluorinated Pyridines Using Tetrabutylammonium Fluoride

By Mobinikhaledi, A. and Foroughifar, N.
From Phosphorus, Sulfur and Silicon and the Related Elements, 181(2), 405-412; 2006

4-(Bromomethyl)-2,6-di-tert-butylpyridine (4a) A mixture of 2,6-di-tert-butyl-4-methylpyridine, 1, (0.21 g, 1.0 mmol), NBS (0.18 g, 1 mmol), and dibenzoyl peroxide (0.025 g, 1 mmol) in dry carbon tetrachloride (15 mL) was refluxed under N2 for 3 h. The mixture was then cooled in an ice bath and the precipitated succinimide was removed by filtration. The solvent was evaporated to give a brown oily mixture. This mixture was dissolved in carbon tetrachloride (15 mL). NBS (0.036 g, 0.20 mmol) and dibenzoyl peroxide (0.0050 g, 0.021 mmol) added and refluxed under N2 for another 2 h. The crude product was distilled at 90-110°C/2 mm Hg to give pure compound 4a (93%). 4-(Bromomethyl)-2,6-di-tert-butylpyridine (4a), yield 93%. 1H NMR (CDCl3): δ (ppm): 1.35 (18H, s, 2 x t-butyl), 4.38 (2H, s, CH2Br), 7.09 (2H, s, Ar). 13C NMR (CDCl3): δ (ppm): 30.1 (2 x t-butyl), 32.2 (CH2Br), 37.7 (2 x C), 115.3 (2 x CH, Ar), 145.7 (1 x C, Ar), 168.4 (2 x C, Ar)，