反应 #1447085

反应方程式

mannobiose

GlcNAc

→

GlcNAc mannobiose

溶剂

CH2Cl2

CH2Cl2

反应条件

后处理

1. 1
   其他Insoluble materials were removed by passage through silica gel
2. 2
   workup.ADDITIONthe filtrate was then diluted with EtOAc
3. 3
   洗涤washed with brine, aq. NaHCO3 and brine successively
4. 4
   干燥dried over Na2SO4
5. 5
   其他evaporated in vacuo
6. 6
   其他The residue was purified by silica gel column chromatography (toluene:EtOAc, 15:1-10:1)

实验过程

To a stirred mixture of Cp2HfCl2 (269.5 mg, 0.710 mmol), AgOTf (365.5 mg, 1.423 mmol), and molecular sieves 4A (3 g) in dry CH2Cl2 (5 mL) was added a solution of mannobiose acceptor (541.1 mg, 0.593 mmol) and GlcNAc-donor (354.0 g, 0.609 mmol) in dry CH2Cl2 (10 mL) at −78° C. The mixture was stirred for 2 h and at −40° C. for 1 h. Insoluble materials were removed by passage through silica gel and the filtrate was then diluted with EtOAc, washed with brine, aq. NaHCO3 and brine successively, dried over Na2SO4, and evaporated in vacuo. The residue was purified by silica gel column chromatography (toluene:EtOAc, 15:1-10:1) to afford compound GlcNAc-mannobiose donor (393.4 mg, 45%).

来源