反应详情

温度

2.5 °C

A mixture of 3-tert-butyl phenol (500.0 mg, 3.33 mmol) and 2-chloro-N-(hydroxymethyl)acetamide (411.2 mg, 3.33 mmol) was added in portions to an ice-bath cold solution of acetic acid (3.0 ml) and conc. H2SO4 (0.5 ml). The mixture was stirred at 0-5° C. for 3.0 h. and then it was allowed to warm to r.t. Stirring continued at r.t. for 20 h. The mixture was poured into ice-water, neutralized with solid NaHCO3 and extracted with CH2Cl2. The combined organic extracts were dried (MgSO4), filtered and concentrated. The crude product was purified by flash chromatography; Pet. Ether, EtOAc (9:1→7:3) affording 278 mg (33%) the title compound.

1. temperatureto warm to r.t
2. stirringStirring
3. waitcontinued at r.t. for 20 h
4. extractionextracted with CH2Cl2
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was purified by flash chromatography