Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Tetrachloride → Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon Tetrachloride | HCID 5943 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate | HCID 136158782 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate | HCID 59394353 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08541432B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-9e9734a2181b49b18187f5c64442815c |
| 출처 메모 | uspto-grants-2013_09 |