참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethylsilyl triflate | HCID 65367 | — |
| 반응물 | 2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane | HCID 81858 | — |
| 반응물 | Methyl 3-oxocyclohexane-1-carboxylate | HCID 566099 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate | HCID 372311 | — |
반응 단계
To a solution of trimethylsilyltrifluoromethanesulfonate (0.034 mL) in dry dichloromethane (5 mL) was added 1,2-bis(trimethylsiloxy)ethane (4.55 mL) followed by methyl 3-oxocyclohexanecarboxylate (2.9 g). The reaction mixture was stirred for 3 hours at −78° C. The reaction mixture was quenched with dry pyridine (0.5 mL), poured into saturated aqueous NaHCO3, and extracted with ether. The ether layer was dried over Na2CO3/Na2SO4. The reaction mixture was concentrated and purified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes to provide the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09174982B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
|---|
| ORD ID | ord-ccab818e9a8847958280b228c5ec5b04 |
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| 출처 메모 | uspto-grants-2015_11 |
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