Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Tetrachloride → tert-Butyl 4-chloro-8-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 | 8-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester | HCID 136158780 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | tert-Butyl 4-chloro-8-methyl-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate | HCID 59394669 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08541432B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-42243e31106248d9ba24c74d8de6858e |
| 출처 메모 | uspto-grants-2013_09 |