Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetonitrile → Benzyl ((1S,3R)-3-aminocyclohexyl)carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Bistrifluoroacetoxyiodobenzene | HCID 12041285 | — |
| 반응물 | Benzyl ((1S,3R)-3-carbamoylcyclohexyl)carbamate | HCID 68007396 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Benzyl ((1S,3R)-3-aminocyclohexyl)carbamate | HCID 69756715 | 75% |
반응 단계
Benzyl N-[(1S,3R)-3-carbamoylcyclohexyl]carbamate, 18d, (9.1 g, 32.9 mmol) was suspended in a mixture of acetonitrile (100 mL) and water (100 mL) and treated with bis(trifluoroacetoxy)iodobenzene (15.5 g, 36.1 mmol). The suspension was allowed to stir at room temperature overnight and was then quenched with 1N HCl (100 mL). After evaporation of the acetonitrile, the acidic aqueous solution was washed with EtOAc (2×150 mL). The pH was adjusted to basic by addition of solid KOH and the resulting emulsion was extracted with EtOAc (3×200 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo to provide product 18e (6.2 g, 75% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08829007B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-7abe82ec62c046489b03a6dce808258d |
| 출처 메모 | uspto-grants-2014_09 |