Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Acetate → HCID 54187452, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 반응물 | (2R,5S)-5-Chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde | HCID 53673807 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 54187452 | HCID 54187452 | 99.1% |
반응 단계
To a solution of (2R,5S)-5-chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde (1.86 g, 4.44 mmol) in MeOH (20 mL) was added ammonium acetate (3.42 g, 44 mmol) and sodium cyanoborohydride (0.195 g, 3.1 mmol). The resulting mixture was stirred overnight at ambient temperature. The reaction was quenched with concentrated hydrochloric acid and concentrated in vacuo. The residue was dissolved in water and basified with aqueous 3N NaOH (pH>10). The product was extracted with dichloromethane (2×) and ethyl acetate (2×). The combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (1.29 g, 69% yield)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06649611B2 |
| 출처 데이터셋 | uspto-grants-2003_11 |
| ORD ID | ord-c4ef7363554341ffa01d88267800552d |
| 출처 메모 | uspto-grants-2003_11 |