反应详情

Methyl 4-Hydroxyphenylacetate (4) (0.83 g) was dissolved in saturated methanolic ammonia (30 ml) and placed in a thick walled tube with Teflon screw cap. The solution was stirred in this sealed tube at room temperature for 72 hours. Reaction mixture was concentrated and redissolved in methanol-chloroform (2:8 volume by volume, 75 ml). No crystallization occurred so the solution was concentrated to half its volume and hexane was added with heating. Cooling to 0° C. gave crystals of 4-Hydroxyphenylacetamide (13) (0.524 g). This was confirmed by spectroscopy--1H NMR (d6DMSO+CF3CO2D) δ 3.23 (s, 2 H), 6.63 (d, 2 H), 7.00 (d, 2 H).

1. customscrew cap
2. customReaction mixture
3. concentrationwas concentrated
4. dissolutionredissolved in methanol-chloroform (2:8 volume by volume, 75 ml)
5. customNo crystallization
6. concentrationwas concentrated to half its volume and hexane
7. additionwas added
8. temperaturewith heating
9. temperatureCooling to 0° C.