Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Pyrrolidone → 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Pyrrolidone | HCID 12025 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate | HCID 14966741 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one | HCID 10900293 | 11.5% |
반응 단계
Pyrrolidin-2-one (720 mg, 8.46 mmol) in DMF (5 mL) was treated with NaH (203 mg, 8.46 mmol) at room temperature. The mixture allowed to stir for 30 min. 1,4-dioxaspiro[4.5]decan-8-yl methanesulfonate (500 mg, 2.12 mmol) from above step A, in DMF (3 mL) was added to the mixture and stirred at 130° C. for 3 h. The mixture was cooled to room temperature, quenched with NH4Cl, and extracted into EtOAc. Washed the EtOAc layer with saturated NaCl, dried over Na2SO4 and evaporated. Purified by silica prep TLC to give 55 mg (11.5%) of 1-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08518969B2 |
| 출처 데이터셋 | uspto-grants-2013_08 |
| ORD ID | ord-2ce2d8c96c8d4a18932ee09386df8c9e |
| 출처 메모 | uspto-grants-2013_08 |