참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 3,4-Dichlorobenzaldehyde | HCID 22710 | — |
| 반응물 | 4-Methylbenzene-1-carboximidamide hydrochloride | HCID 122753 | — |
| 반응물 | 3-Phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate | HCID 22005512 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 22005533 | HCID 22005533 | 0.3% |
반응 단계
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]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06218538B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_04 |
|---|
| ORD ID | ord-724a4bcc26cb429cb1cdfa52a6677272 |
|---|
| 출처 메모 | uspto-grants-2001_04 |
|---|
