将无水甲醇（19.2g，0.6 mol)和无水苯40 mL的混合物、在30-40分钟内，滴入ClSO2NCO（85g ，52.3 mL, 0.6 mol)和无水苯200 mL的混合物中，控温10-15℃。加毕，室温搅拌2小时。然后加入1000 mL无水苯稀释后，小心滴入190 mL无水三乙胺和250 mL无水苯的混合物中，控温10-15℃，约40分钟左右加完。加毕，室温搅拌2小时，析出大量固体。反应毕，过滤，固体用无水苯200 mL、无水THF200 mL洗后，滤液浓缩后，（控温<30℃），加入无水THF溶解后，重结晶得123g, 收率86%。注：整个操作温度要低于30℃。
WO2012054510 A1
WO2013017657 A1
WO2017191000 A1
WO2010072746 A1
Organic Letters (2016), 18(3), 460-463
2.2 Burgess试剂用酰胺脱水合成腈
WO2016075239 A1
Burgess reagent (1.7 g, 7.19 mmol) is added to a solution
of 6a (840 mg, 4.79 mmol) in DCM (15 mL), and
the mixture is heated for 3h at 35°C. The reaction is diluted with DCM, washed
with 0.2N hydrochloric acid and brine. The organic layer is separated and dried
with a Phase separator cartridge and evaporated under vacuum to obtain a crude
that is purified by flash chromatography (eluent 0-20% EtOAc/cyclohexane) to
furnish the title compound (680 mg, 90%).WO2011071570 A1
Journal of Medicinal Chemistry (2014), 57(6), 2357-2367
WO2013041497 A1
European
Journal of Organic Chemistry (2018), 2018(45), 6256-6273
At room temp.
(methoxycarbonylsulfamoyl)triethylammonium hydroxide inner salt (Burgess
reagent, 194 mg,813 µmol, 3.0 equiv.) was
added to a solution of the hydroxycyclopentanone cis-39
(121 mg, 271 µmol) in toluene (3 mL). The mixture was stirred at 100°C for 12 h and then cooled to room temp. Silica
gel was added and the solvent was evaporated under reduced pressure.
Purification by flash chromatography afforded
compound cis-40 (113 mg, 263 µmol, 97%) as a white solidJournal of Organic Chemistry (2016), 81(22),
11017-11034
WO2016015014 A1
To a stirring mixture of
8-(4-propylphenyl)-l,4-dioxaspiro[4.5]decan-8- ol (1.38
g, 4.99 mmol) in THF (24 mL) was added Burgess
reagent (2.38 g, 9.99 mmol). The mixture was heated at 50°C for 3 h. The solvent was evaporated and the 15
reaction mixture partitioned between water (30 mL) and DCM (50 mL). Solvents
were evaporated and the residue purified by column chromatographyto afford 1.21 g (93%) of
8-(4-propylphenyl)-1,4-dioxaspiro[4.5]dec-7-ene (1.21 g, 4.64 mmol, 93 % yield)
as a colourless oil.Organic & Biomolecular Chemistry (2017), 15(20), 4282-4285
The respective alcohol (200
µmol) was dissolved in 1,4-dioxane (1.0 mL). Burgess' reagent (96.0 mg, 400 µmol) was added, the
reaction vial was sealed with a septum and submitted to the microwave reactor. The reaction mixture was irradiated
for 1 minute with a capacity of 150 W to reach a temperature of 150 °C. The reaction was stirred for 3 minutes at
this temperature and then cooled down to ambient temperature. The reaction
mixture was directly subjected to silica gel flash chromatography using
petroleum ether/EtOAc (using the solvent composition or gradient indicated) for
purification of the crude product.2.4 Burgess试剂用于醇的氧化
J. Org. Chem. 2017, 82, 2, 1046–1052
在本文中，我们发现，在二甲亚砜溶剂下，Burgess试剂有效且快速地促进广泛的伯醇和仲醇以优异的产率和温和的条件下氧化为其相应的醛和酮。而在其他溶剂中反应是羟基脱水。
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