Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-Oxo-4-pyrimidin-2-yl-piperazine-1-carboxylic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-Bromopyrimidine | HCID 78345 | — |
| 반응물 | Tert-butyl 3-oxopiperazine-1-carboxylate | HCID 3157178 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-Oxo-4-pyrimidin-2-yl-piperazine-1-carboxylic acid tert-butyl ester | HCID 66823688 | 22.1% |
반응 단계
To 1-Boc-3-oxopiperazine 3a (390 mg, 1.95 mmol) in DMF (5 mL) at 0° C. was added NaH (60% in oil, 97 mg, 2.44 mmol). The reaction was stirred at 0° C. for 25 min before a solution of 2-bromopyrimidine 1i (465 mg, 2.92 mmol) in DMF (2 mL) was added. The reaction was slowly warmed up to room temperature overnight. To the reaction mixture was added H2O, and the resulting mixture was extracted with EtOAc. The organic solution was washed with aq. NaCl, dried over Na2SO4 and concentrated. Purification by column chromatography (silica gel, 3% MeOH/CH2Cl2) gave 3b as yellow oil (120 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08637498B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-fc838a80b82e4d749e867ac2a3ccc6be |
| 출처 메모 | uspto-grants-2014_01 |