関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl Acrylate | HCID 8821 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (2R)-(-)-2-Methylpyrrolidine hydrochloride | HCID 11147704 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(2-(R)-Methyl-pyrrolidin-1-yl)-propionic acid ethyl ester | HCID 59696738 | 100.8% |
反応手順
In a round-bottom flask, 2-(R)-methylpyrrolidine HCl (5.5 g, 45 mmol) was dissolved in CH3CN (20 mL). To the stirred solution was added milled K2CO3 (8.3 g, 60 mmol). The suspension was stirred at room temperature for approximately 1 h. Ethyl acrylate (3.25 mL, 30 mmol) and EtOH (40 mL) were then added. The reaction mixture was stirred until analysis by GC showed completion (the Area % of ethyl acrylate was less than 1% (approximately 2 h)). The reaction mixture was filtered and the wet cake (excess K2CO3) was washed with CH3CN (5–10 mL). The filtered solution was then concentrated under reduced pressure to minimum volume (white slurry). Methyl t-butyl ether (MTBE) and H2O were added, at which time all solids dissolved. The organic layer was washed a second time with water and then concentrated to yield 5.6 g of the title compound. The oil product was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094790B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-fec01abb86294747961ee324773560ef |
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| 出典メモ | uspto-grants-2006_08 |
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