참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 반응물 | 4-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole | HCID 14735629 | — |
| 반응물 | HCID 178418373 | HCID 178418373 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | HCID 20284777 | HCID 20284777 | — |
반응 단계
Methyl magnesium iodide prepared from reaction of magnesium (2.4 g) and methyl iodide (13.9 g) in absolute ether is dissolved in absolute benzene (50 ml) and a solution of 4-formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole (5.5 g) in absolute benzene (60 ml) is added dropwise thereto during 3 hours. The mixture is stirred at room temperature for 1 hour, poured slowly into an ice water containing ammonium chloride (10 g) and extracted with ether. The extract is evaporated. The oily residue is chromatographed on a column of silica gel and eluted with ether-benzene (1:50). The eluate is evaporated. The residue is again chromatographed on a column of silica gel and eluted with benzene and ether-benzene (1:20). The title compound is obtained from the latter eluate as an oil (4.58 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04256640 |
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| 출처 데이터셋 | uspto-grants-1981_03 |
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| ORD ID | ord-c88c20fec02f4ae395639a69a822b0fe |
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| 출처 메모 | uspto-grants-1981_03 |
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