HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Tetrachloride → tert-Butyl 4-chloro-8-methyl-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 8-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester | HCID 136158780 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | tert-Butyl 4-chloro-8-methyl-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate | HCID 59394669 | — |
Reaction Steps
A combination of 8-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester (374 mg, 1.41 mmol), triphenylphosphine (739 mg, 2.82 mmol) and carbon tetrachloride (409 uL, 4.23 mmol) and 1,2-DCE (10 mL) are heated at 70° C. for 6 h. The solution is then concentrated in vacuo and the residue separated via FCC (5-60% EtOAc/heptane). MS (ESI) m/z 284.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08242125B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-4abadd860c65495abafc37c773c4642d |
| Source note | uspto-grants-2012_08 |