反应详情

To a cooled (−78° C.) solution of oxalyl chloride in CH2Cl2 (15 mL, 1M) is added, dropwise, DMSO (3 mL). The resulting solution is stirred for 5 minutes then a solution of 4-[pyridin-4-yl]-benzyl alcohol (2.80 g, 15 mmol) (reference example 13a) in CH2Cl2/DMSO (27 mL, 3:1 CH2Cl2/DMSO) is added dropwise. The resulting mixture is stirred 5 minutes then Et3N added (15 mL, 108 mmol) in one portion. The cold bath is removed and stirring continued for 15 minutes. The reaction mixture is then diluted with ethyl acetate, washed with water and then brine, dried over MgSO4 and concentrated. The crude, orange solid product is used without further purification.

1. additionis added
2. stirringThe resulting mixture is stirred 5 minutes
3. customThe cold bath is removed
4. stirringstirring
5. waitcontinued for 15 minutes
6. additionThe reaction mixture is then diluted with ethyl acetate
7. washwashed with water
8. dry with materialbrine, dried over MgSO4
9. concentrationconcentrated
10. customThe crude, orange solid product is used without further purification