Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 6-benzyl-3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 10016028 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 10241423 | 179.8% |
반응 단계
A solution of 96 g of 6-benzyl-3-methyl-5,6,7,8-tetra-hydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione from c) in 1.5 1 of glacial acetic acid was debenzylated by hydrogenolysis for 6 h on 14.6 g of 10% palladium/activated charcoal at 25° C. and 3.5 bar. After the catalyst had been filtered off, the filtrate was concentrated under reduced pressure. The above preparation was repeated. The two crude products were combined, dissolved in water and precipitated, with stirring, by the addition of 33% sodium hydroxide solution to pH 6.9. The precipitate was washed with water and dried at 60° C. under reduced pressure to give 115.3 g of 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05556854 |
| 출처 데이터셋 | uspto-grants-1996_09 |
| ORD ID | ord-9554e01e27824ec083075b202565eeed |
| 출처 메모 | uspto-grants-1996_09 |