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Carbon Tetrachloride → Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate | HCID 136158782 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate | HCID 59394353 | — |
反応手順
A solution of (±)-6-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester, (7.5 g, 28.3 mmol), triphenylphosphine (14.8 g, 56.5 mmol) and carbon tetrachloride (8.2 mL, 85 mmol) in 1,2-DCE (100 mL) is heated at 80° C. for 6 h. At that time the solution is concentrated in vacuo and the residue is separated via FCC (5-60% EtOAc/heptane) to give the title compound. MS (ESI) m/z 284.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486954B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-7d1da397b7c344d8b5ebb2b31d846876 |
| 出典メモ | uspto-grants-2013_07 |