Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-[2,2-Bis-(4-chloro-phenyl)-ethyl]-piperazine-1-carboxylic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 반응물 | Bis(4-chlorophenyl)acetaldehyde | HCID 167694 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 4-[2,2-Bis-(4-chloro-phenyl)-ethyl]-piperazine-1-carboxylic acid tert-butyl ester | HCID 59331952 | 11.1% |
반응 단계
To a solution of bis-(4-chloro-phenyl)-acetaldehyde (3.74 mmol) in methanol under a nitrogen atmosphere, N-BOC-piperazine (1.05 g, 5.61 mmol) was added ???, the reaction mixture was stirred for 1 hour before addition of sodium cyanoborohydride (0.28 g, 4.49 mmol). The reaction mixture was stirred for 18 hours, water added (3 ml) and the solvent removed under reduced pressure. The residue was partitioned between dichloromethane and water, the organic layer was separated, dried (MgSO4), filtered and concentrated. Purified over flash silica chromatography eluting with ethyl acetate/petroleum ether (3:7) to yield the title compound (0.18 g, 11% yield for steps 30A and 30B combined). LC/MS: (PS-A2) Rt 2.66 E[M−BOC+H]+ 335.02.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08247576B2 |
| 출처 데이터셋 | uspto-grants-2012_08 |
| ORD ID | ord-7fee586c4edc4e46b3a36d20e6e7ad15 |
| 출처 메모 | uspto-grants-2012_08 |