참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 반응물 | 4-Hydroxy-5,5-dimethyl-2(5H)-furanone | HCID 54720139 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,2-Dimethyl-5-oxo-2,5-dihydrofuran-3-yl trifluoromethanesulfonate | HCID 58926348 | 89% |
반응 단계
To a −78° C. stirred solution of 4-hydroxy-5,5-dimethyl-5H-furan-2-one (250 mg, 1.95 mmol) in 18 mL of anhydrous CH2Cl2, was added triethylamine (0.40 mL, 2.9 mmol) and Tf2O (0.49 mL, 2.9 mmol). The reaction was stirred at −78° C. for 30 minutes, and quenched with saturated NH4Cl solution (10 mL). The mixture was warmed up to room temperature and separated. The aqueous layer was extracted with CH2Cl2 (2×20 mL). All organic layers were combined, dried over Na2SO4 and evaporated to brown oil, which was purified by plugging through a short pad of silica gel column with EtOAc/hexanes (1/3). Evaporation of solvents gave 2,2-dimethyl-5-oxo-2,5-dihydrofuran-3-yl trifluoromethanesulfonate as a light brown oil (450 mg, 89%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08865682B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_10 |
|---|
| ORD ID | ord-dbf4dfca10f742b8b68d1a2721a6fb16 |
|---|
| 출처 메모 | uspto-grants-2014_10 |
|---|