反应详情

温度

60 °C

Crude erlotinib hydrochloride (100 gm, obtained in reference example 1), water (400 ml) and ethyl acetate (1600 ml) are taken into a reaction flask at 25-30° C. and start stirring. The contents are heated to 60° C., pH of the mass is adjusted to 9 to 10 by adding sodium hydroxide solution (30-40 ml) at 60-65° C. and then stirred for 30-35 minutes at 60-65° C. Separated the layers at 60-65° C., the organic layer is dried with sodium sulfate and then distilled off the solvent completely under vacuum at 50° C. The residue is cooled to 25-30° C., n-heptane (800 ml) is added and the stirred for 45 minutes to 1 hour at 25-30° C. Filtered the compound, washed with n-heptane (200 ml) and then dried at 60-65° C. to give 90 gm of anhydrous erlotinib free base (HPLC Purity: 99.1%, Moisture Content: 0.1%).

1. stirringstirred for 30-35 minutes at 60-65° C
2. customSeparated the layers at 60-65° C.
3. dry with materialthe organic layer is dried with sodium sulfate
4. distillationdistilled off the solvent completely under vacuum at 50° C
5. temperatureThe residue is cooled to 25-30° C.
6. additionn-heptane (800 ml) is added
7. stirringthe stirred for 45 minutes to 1 hour at 25-30° C
8. filtrationFiltered the compound
9. washwashed with n-heptane (200 ml)
10. customdried at 60-65° C.