Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione | HCID 13072423 | — |
| 반응물 | Sodium methanolate methanol | HCID 23694274 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine | HCID 21323406 | — |
반응 단계
To 3 ml of methanol was added 0.215 g of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione and, under stirring, 0.6 ml of 2N-sodium methoxide/methanol was added. Then, 0.07 ml of methyl iodide was added dropwise. After 20 minutes, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with ether. In this manner, 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine were obtained as crystals. Recrystallization from methanol yielded colorless needles melting at 168°-169° C. This was identical with the products obtained in Examples 1 and 2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04150139 |
| 출처 데이터셋 | uspto-grants-1979_04 |
| ORD ID | ord-bab0281336fd44af883de71d8461ae1f |
| 출처 메모 | uspto-grants-1979_04 |