Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 5-(N-ethylsulfonyl-N-methylamino)-2,3,4,5-tetrahydro-1-benzoxepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 5-Ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine | HCID 22391808 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(N-ethylsulfonyl-N-methylamino)-2,3,4,5-tetrahydro-1-benzoxepine | HCID 15434533 | 95.2% |
반응 단계
A solution of 1.0 g (3.9 mmol) of 5-ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine in 15 ml of THF were added dropwise under nitrogen to a suspension of 0.16 g (5.4 mmol) of 80 percent sodium hydride in 10 ml of THF. After stirring at RT for 3 h, 1.6 g (11 mmol) of methyl iodide were added dropwise and the mixture was additionally stirred overnight at RT. After distilling off the solvent, the residue was treated with water and extracted with EA. The organic phase was concentrated in vacuo after drying over sodium sulfate. 1.0 g of 5-(N-ethylsulfonyl-N-methylamino)-2,3,4,5-tetrahydro-1-benzoxepine was obtained, m.p. 122-124° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06333349B1 |
| 출처 데이터셋 | uspto-grants-2001_12 |
| ORD ID | ord-a6dc94c4fe4b4a9fbe05f414a473c68f |
| 출처 메모 | uspto-grants-2001_12 |