関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl acetoacetate | HCID 7757 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 3-tetrahydropyrrolyl-2-butenoate | HCID 69630084 | 99.5% |
反応手順
Methyl acetoacetate (20 g, 172.23 mmol) was dissolved in 250 mL of toluene, and then pyrrolidine (43 ml, 516.70 mmol) and p-toluenesulfonic acid hydrate (about 100 mg) were added dropwise. After installing a Dean-Stark separator to the reactor, the reaction mixture was refluxed 140° C. for two days, and then solvent was removed by concentrating the resulting mixture under a reduced pressure, thereby to obtain the desired product (29 g, 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07094908B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-8ef35b9c9c5c40bcabb7b408e1cb86f0 |
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| 出典メモ | uspto-grants-2006_08 |
|---|
