Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HCID 54224365, 화합물 → (1R,4R,5S)-6,6-dimethyl-2-oxo-4-trichloromethyl-3-oxabicyclo[3.1.0]hexane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | HCID 54224365 | HCID 54224365 | — |
| 촉매 | Bis(pentane-2,4-dione-kappa~2~O~2~,O~4~)copper | HCID 45052134 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (1R,4R,5S)-6,6-dimethyl-2-oxo-4-trichloromethyl-3-oxabicyclo[3.1.0]hexane | HCID 10538220 | 90% |
반응 단계
A solution of (1R)-3-methyl-1-trichloromethyl-2-butenyl diazoacetate (0.90 g, 3.33 mmole) from Example IA.4.(a) in 15 ml of dry dioxane was added dropwise over a period of 2.6 hours to a catalytic amount (approximately 2 mole %) of cupric acetylacetonate in 65 ml of refluxing dry dioxane under a nitrogen atmosphere. After refluxing for an additional hour, the mixture was evaporated, and an etheral solution of the residue was washed with 1 N HCl, saturated NaHCO3, and saturated NaCl, then dried over MgSO4 and evaporated to give (1R,4R,5S)-6,6-dimethyl-2-oxo-4-trichloromethyl-3-oxabicyclo[3.1.0]hexane (0.73 g, 90% crude yield) as a green-yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04254282 |
| 출처 데이터셋 | uspto-grants-1981_03 |
| ORD ID | ord-c0357354741542c28358447386ef9bb0 |
| 출처 메모 | uspto-grants-1981_03 |