참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyloxyamine hydrochloride | HCID 102312 | — |
| 반응물 | 5'-Bromo-2'-(methylthio)spiro[cyclohexane-1,3'-[3H]indole] | HCID 21986266 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178419047 | HCID 178419047 | — |
반응 단계
5′-Bromo-2′-(methylthio)spiro[cyclohexane-1,3′-[3H]indole] (9.0 g, 28.98 mmol) and O-benzylhydroxylamine hydrochloride (13.8 g, 86.9 mmol) were combined in methanol (150 mL) and heated to 45° C. for 6 hours. Methanol was evaporated in vacuo. Ethyl acetate was added to the residue and this mixture was washed with ammonium chloride solution. Ethyl acetate was dried over magnesium sulfate, ethyl acetate collected evaporated in vacuo and the residue was flash chromatographed on alumina 90 (9:1 Hexane/EtOAc) to the desired product (6.5 g, 60%). 1H NMR (DMSO-d6, 300 MHz) δ 1.38–1.70 (m, 8H), 1.92–2.06 (m, 2H), 5.06 (s, 2H), 6.71 (d, 1H, J=8.26 Hz), 7.22–7.43 (m, 7H), 9.62 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07091234B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-2a5db7c4f64e47bcb8b812a4d9f7db0b |
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| 출처 메모 | uspto-grants-2006_08 |
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