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Toluene → HCID 178469205、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | 4-Phenylcyclohexanol | HCID 79497 | — |
| 反応物 | Ethyl 1-((6-hydroxynaphthalen-2-yl)methyl)piperidine-4-carboxylate | HCID 68279222 | — |
| 生成物 | HCID 178469205 | HCID 178469205 | 50% |
反応手順
A mixture of 1-(6-hydroxy-naphthalen-2-ylmethyl)-piperidine-4-carboxylic acid ethyl ester (0.400 g, 1.28 mmol), 4-phenyl-cyclohexanol (0.2479 g, 1.406 mmol) and triphenylphosphine (0.6695 g, 2.553 mmol) in toluene (5 mL, 40 mmol) was stirred for 20 min, then diisopropyl azodicarboxylate (0.32 mL, 1.5 mmol) was added dropwise at 0° C. The solution was stirred at reflux overnight. The reaction was added silica gel and the solvent was concentrated. The residue was purified with silica gel eluted with EtOAc in hexanes from 0 to 20% to give product as an oil (0.3 g, 50%). LCMS: Rt=1.75 min, m/z=472.45 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09340527B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-5f1015eb4a024fe496a210a4adf75146 |
| 出典メモ | uspto-grants-2016_05 |