Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfate → 1,3-Dihydro-4-methoxy-1,3-dimethyl-2H-indol-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,3-dihydro-4-hydroxy-1,3-dimethyl-2H-indol-2-one | HCID 19692945 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 1,3-Dihydro-4-methoxy-1,3-dimethyl-2H-indol-2-one | HCID 19692955 | 86.2% |
반응 단계
A slurry of 1,3-dihydro-4-hydroxy-1,3-dimethyl-2H-indol-2-one (50 g), milled potassium carbonate (60.1 g) and HPLC grade acetone (400 ml) was mechanically stirred at room temperature as dimethylsulfate (41.4 ml) was added dropwise. The addition funnel was replaced with a condenser and the slurry was refluxed for 18 hours. The K2CO3 was filtered off and washed well with acetone. Acetone was evaporated and the residue was purified by column chromatography to yield 46.5 g of an oil. The oil was dissolved in ether and placed in the refrigerator where, upon standing overnight, the product crystallized, m.p. 73°-74° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05726323 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-0f8c43802c60460ab93e17f76623a594 |
| 출처 메모 | uspto-grants-1998_03 |