Acetic Anhydride → HCID 11367118、化合物

温度

200 °C

1,3-Cyclohexanedicarboxylic acid (mixture of cis and trans; 20 g; 0.116 mol) was slurried in acetic anhydride (80 mL; 0.85 mol; 7.3 equiv). The resulting mixture was heated to reflux (at which point it was homogeneous) for 5 h. A distillation head was added and the volatiles were removed by increasing the pot temperature to 200° C. Once no more distillate was collected the residue was cooled to ambient temperature to afford a solid mass. The crude product was recrystallized from hot toluene (40 mL) by the addition of heptane (40 mL) and cooling to 4° C. The precipitated product was filtered, washed with heptane, and dried in vacuo to afford 16.74 g (93%) of 1.

1. temperatureThe resulting mixture was heated
2. temperatureto reflux (at which point it was homogeneous) for 5 h
3. additionA distillation head was added
4. customthe volatiles were removed
5. distillationOnce no more distillate was collected the residue
6. temperaturewas cooled to ambient temperature
7. customto afford a solid mass
8. customThe crude product was recrystallized from hot toluene (40 mL) by the addition of heptane (40 mL)
9. temperaturecooling to 4° C
10. filtrationThe precipitated product was filtered
11. washwashed with heptane
12. customdried in vacuo

ORDレコード

ord-cd02d1efe2e8498d805a934276ba4f2b

出典データセット

uspto-grants-2000_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06028213