Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 6-Bromo-3 4-dihydro-4,4-dimethyl-8-vinylspiro[2H-1-benzopyran-2,1'-cyclopropane]
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Methylenetriphenylphosphorane | HCID 137960 | — |
| 반응물 | 6-bromo-8-carbonyl-3,4-dihydro-4,4-dimethylspiro [2H-1-benzopyran-2,1'-cyclopropane] | HCID 18177968 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 6-Bromo-3 4-dihydro-4,4-dimethyl-8-vinylspiro[2H-1-benzopyran-2,1'-cyclopropane] | HCID 22568855 | — |
반응 단계
Following general procedure N and using A solution of methylidene triphenyl phosphorane [generated from methyl triphenylphosphonium bromide (7 g, 20 mmol) and 1.6M solution of n-butyl lithium in hexanes (11.8 mL, 19 mmol)], 6-bromo-8-carbonyl-3,4-dihydro-4,4-dimethylspiro[2H-1-benzopyran-2,1′-cyclopropane](Intermediate 40, 2.06 g, 7 mmol) followed by flash column chromatography over silica gel (230-400 mesh) using 1-2% ethyl acetate in hexane as the eluent, the title compound was obtained as a clear oil (1.36 g, 66%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06855512B2 |
| 출처 데이터셋 | uspto-grants-2005_02 |
| ORD ID | ord-32d9f729b81e4268b027aedee27a797c |
| 출처 메모 | uspto-grants-2005_02 |