関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 3,4-Dichlorobenzaldehyde | HCID 22710 | — |
| 反応物 | 4-Methylbenzene-1-carboximidamide hydrochloride | HCID 122753 | — |
| 反応物 | 3-Phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate | HCID 22005512 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 22005533 | HCID 22005533 | 0.3% |
反応手順
A mixture of 3-phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate (7.9 g, 22.7 mmol), 3,4-dichlorobenzaldehyde (4.0 g, 22.7 mmol), p-toluamidine hydrochloride (3.87 g, 22.7 mmol) and glacial acetic acid (1.3 mL, 22.7 mmol) was stirred in N,N-dimethylformamide (40 ml) for 2 days at room temperature and then heated to 60° C. for 7 days. The DMF was removed in vacuo and ethyl acetate was added to the residue. The precipitate was removed by filtration and the filtrate was washed with water, sodium hydrogen carbonate solution and brine, dried and evaporated to yield an oil. The oil was further purified by flash chromatography and RP-HPLC to give the title compound (45 mg) as an oil. Electrospray MS m/z 620/622 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06218538B1 |
|---|
| 出典データセット | uspto-grants-2001_04 |
|---|
| ORD ID | ord-724a4bcc26cb429cb1cdfa52a6677272 |
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| 出典メモ | uspto-grants-2001_04 |
|---|
