Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4,7-Dimethyl-5-methoxy-3-(methylthio)-1,3-dihydro-2H-indol-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Sulfuryl chloride | HCID 24648 | — |
| 반응물 | Methyl (methylthio)acetate | HCID 85522 | — |
| 반응물 | Proton sponge | HCID 88675 | — |
| 반응물 | 4-Methoxy-2,5-dimethylaniline | HCID 22506864 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4,7-Dimethyl-5-methoxy-3-(methylthio)-1,3-dihydro-2H-indol-2-one | HCID 22506877 | 77.1% |
반응 단계
To a solution of methyl (methylthio)acetate (14.8 ml, 115 mmol) in dichloromethane (400 ml) was added sulfuryl chloride (9.64 ml, 120 mmol) at −78° C. and stirred for 15 minutes. To the mixture was added dropwise a solution of 4-methoxy-2,5-dimethylaniline (15.1 g, 100 mmol) and proton sponge (22.5 g, 105 mmol) in dichloromethane (100 ml) over 1 hour and the mixture was stirred at the same temperature for 1 hour. Then, triethylamine (15.3 ml, 110 mmol) was added, and the mixture was allowed to warm to room temperature slowly. After stirring at room temperature for 1 hour, water was added and the precipitated crystals were collected by filtration and washed with dichloromethane and water to obtain 18.3 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06872718B1 |
| 출처 데이터셋 | uspto-grants-2005_03 |
| ORD ID | ord-5a37714130484af88bbda379de5341ac |
| 출처 메모 | uspto-grants-2005_03 |