反应详情

Phenol (13.1 moles) was heated to 150° and stirred under N2 as 2-ethyl-2-oxazoline (12.2 moles) was added over 1 hr. The mixture was heated to 175±3°. After heating 16 hr the oil was cooled to about 140°, and then it was poured into water (12 L) with vigorous stirring. The mixture was stirred and cooled, and at about 25° the mixture was seeded with crystalline amide product. The material solidified and the supernatant was decanted. The residual solid was stirred with 17 L of hot (85°) water. The mixture was cooled to 25°, seeded with the amide product, and the mixture refrigerated. The resulting granular solid was collected on a filter, rinsed with several portions of water and left to air dry. This gave a 92% yield of material, m.p. 61.5°-64°.

1. additionwas added over 1 hr
2. temperatureThe mixture was heated to 175±3°
3. temperatureAfter heating 16 hr the oil
4. temperaturewas cooled to about 140°
5. temperaturecooled
6. customat about 25°
7. customthe supernatant was decanted
8. stirringThe residual solid was stirred with 17 L of hot (85°) water
9. temperatureThe mixture was cooled to 25°
10. customThe resulting granular solid was collected on a filter
11. washrinsed with several portions of water
12. waitleft to air
13. customdry