Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → HCID 59240648, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Benzyl-4-chlorophthalazine | HCID 6404566 | — |
| 반응물 | (S)-4-(5-Methoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl-ester | HCID 68707290 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 59240648 | HCID 59240648 | 8% |
반응 단계
To a methylene chloride (0.02M) solution of (S)-4-(5-Methoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl-ester (69 mg, 0.153 mmol), is added 1N HCl (2 mmol), 2M in diethyl ether. Stir reaction mixture at room temperature for 18 h. Concentrate and dilute with dioxane (0.1 M), followed by addition of 1-benzyl-4-chloro-phthalazine (0.153 mmol) and triethylamine (0.459 mmol). Microwave reaction mixture for 30 min at 150° C. MS shows some starting material still present. Microwave for an additional 2.5 h at 150° C. Concentrate reaction mixture and purify by column chromatography 0-75% ethyl acetate/heptane gradient to afford the title compound. (8% yield)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536168B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-1fb9fdad713d49a7b704ceef49f7cac2 |
| 출처 메모 | uspto-grants-2013_09 |