Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Methyl (3RS)-2-[(methylthio)thiocarbonyl]-1,2,3,4-tetrahydro-beta-carboline-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,3,4,9-Tetrahydro-1H-beta-carboline-3-carboxylic acid methyl ester | HCID 177728 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Methyl (3RS)-2-[(methylthio)thiocarbonyl]-1,2,3,4-tetrahydro-beta-carboline-3-carboxylate | HCID 13561978 | 65.6% |
반응 단계
Methyl (3RS)-1,2,3,4-tetrahydro-β-carboline-3-carboxylate (2.30 g) is dissolved in methanol (50 ml) and thereto are added triethylamine (1.21 g) and carbon disulfide (920 mg). The mixture is stirred at room temperature for 20 minutes and thereto is added dropwise methyl iodide (1.70 g). The mixture is stirred for 4 hours and distilled under reduced pressure to remove the solvent. The residue is dissolved in ethyl acetate, and the mixture is washed with water, dried and distilled to remove the solvent. The residue is recrystallized from ether-n-hexane to give the title compound (2.10 g, 65.6%) as colorless needles, m.p. 132°-134° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04628057 |
| 출처 데이터셋 | uspto-grants-1986_12 |
| ORD ID | ord-836bbc67d48f436686a50a33da215470 |
| 출처 메모 | uspto-grants-1986_12 |