Preparation method and intermediate of fused tricyclic derivative
A compound and mixture technology, applied in the field of medicine, can solve problems such as low safety, abused patients, and dependence
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Embodiment 1
[0115]
[0116] The first step: cyclopent-3-en-1-ylbenzenesulfonate (1-2)
[0117]
[0118] Dissolve cyclopent-3-en-1-ol (5 g, 59 mmol) in dichloromethane (150 mL) and cool to 0°C. Triethylamine (14 mL) was added, and phenylsulfonyl chloride (12.6 g, 71 mmol) was added dropwise. Natural heating. Stir for 1 hour. Cool to 0°C, adjust the pH to about 4 with concentrated hydrochloric acid, and add water (100ml). Extracted with ethyl acetate (150 mL×3). Dry (anhydrous sodium sulfate), spin dry. The residue was separated and purified by column chromatography (petroleum ether / ethyl acetate=10:1) to obtain cyclopent-3-en-1-ylbenzenesulfonate 1-2 (11.5 g, yield 86.3%), 1 H NMR (400MHz, CDCl 3 )δ7.95–7.86(m,2H),7.68–7.60(m,1H),7.56(d,J=7.9Hz,2H),5.71–5.60(m,2H),5.25–5.13(m,1H) ,2.71–2.42(m,4H).
[0119] The second step: ethyl 4-(cyclopent-3-en-1-yl)-3-oxobutyrate (1-3)
[0120]
[0121] Sodium hydride (0.43 g, 11 mmol, 60%) was put into dry THF (15 mL), protected by ni...
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