関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | pyridine TFA | HCID 9813011 | — |
| 反応物 | 7-(2-Hydroxymethyl-6-oxo-piperidin-1-yl)-hept-5-ynoic acid methyl ester | HCID 69020340 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 7-(2-Formyl-6-oxo-piperidin-1-yl)-hept-5-ynoic acid methyl ester | HCID 86012500 | — |
反応手順
1-(3-(Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI, 530 mg, 2.76 mmol) and DMSO (0.26 mL, 3.68 mmol) were added sequentially to a solution of 7-(2-hydroxymethyl-6-oxo-piperidin-1-yl)-hept-5-ynoic acid methyl ester (246 mg, 0.92 mmol) in benzene (7.0 mL) at rt. The mixture was cooled to 0° C. and pyridinium trifluoroacetate (196 mg, 1.01 mmol) was added. The reaction was allowed to warm to rt and then was stirred at rt for 2.5 h. The solution was decanted from the oily residue and the residue was washed with benzene (3×5 mL). The combined benzene phases were concentrated in vacuo to afford crude 7-(2-formyl-6-oxo-piperidin-1-yl)-hept-5-ynoic acid methyl ester that was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06747037B1 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-f0eea8d402f548e19a0d32a705e989b7 |
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| 出典メモ | uspto-grants-2004_06 |
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