反応 #1447085

反応方程式

mannobiose

GlcNAc

→

GlcNAc mannobiose

溶媒

CH2Cl2

CH2Cl2

反応条件

後処理

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

実験手順

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%).

出典