Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-(3-Methyl-2-nitrophenyl)-piperazine-1-carboxylic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 반응물 | 3-Methyl-2-nitrophenyl trifluoromethanesulphonate | HCID 15869552 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 4-(3-Methyl-2-nitrophenyl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 60108775 | 37.5% |
반응 단계
Trifluoromethanesulfonic acid 3-methyl-2-nitrophenyl ester (26.7 g, 93.6 mmol), 1-tert-butoxycarbonyl piperazine (17 g, 91.3 mmol) and triethylamine (14 mL, 100 mmol) in 250 mL of acetonitrile was heated under reflux for 25 h. The mixture was concentrated in vacuo, diluted with water and extracted with ether. The ether was washed with aqueous ammonium hydroxide and brine, dried, and evaporated. Purification by silica gel chromatography (10% ethyl acetate-hexane) afforded 11 g of 4-(3-methyl-2-nitrophenyl)-piperazine-1-carboxylic acid tert-butyl ester as a golden solid, m.p. 101-102° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06787535B2 |
| 출처 데이터셋 | uspto-grants-2004_09 |
| ORD ID | ord-fef11ca5a52242f8bab6da1a7db8c076 |
| 출처 메모 | uspto-grants-2004_09 |