HuagongsheHuagongshe Chemistry Print Report · For research reference only
Calcium Carbonate → Afatinib Impurity 56
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Calcium Carbonate | HCID 10112 | — |
| Reactant | HCID 15079752 | HCID 15079752 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Afatinib Impurity 56 | HCID 59504961 | 39.4% |
Reaction Steps
2 g of the compound obtained in step 1) was diluted with 120 ml of a mixed solvent of ethyl acetate and methanol (1:1), and 450 mg of calcium carbonate on palladium was added thereto. The resulting mixture was stirred under a hydrogen gas for two hours. After the reaction terminated, the resulting solution was filtered through a cellite pad and distilled under a reduced pressure. The resulting residue was purified by column chromatography (methylene chloride:methanol=2:1) to obtain the title compound (800 mg, 39%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188102B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-e45c468293b94d2e840300a46cbb77cd |
| Source note | uspto-grants-2012_05 |