참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | 3-Nitro-p-tolualdehyde | HCID 1798998 | — |
| 반응물 | Furan-2-carboximidamide hydrochloride | HCID 12231049 | — |
| 반응물 | 3-Phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate | HCID 22005512 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 22005532 | HCID 22005532 | 0.9% |
반응 단계
A mixture of 3-phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate (10.0 g, 28.78 mmol), 4-methyl-3-nitrobenzaldehyde (4.75 g, 28.78 mmol), 2-amidinofuran hydrochloride (4.20 g, 28.78 mmol), morpholine (3.75 ml, 43.17 mmol), acetic acid (3.29 ml, 57.56 mmol), and sodium sulfate (8.17 g, 57.56 mmol) was stirred in ethanol (50 ml) for 1 hour at room temperature and then heated to 50° C. for 7 days. The ethanol was removed in vacuo and ethyl acetate was added to the residue. The mixture was filtered 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 (twice) to give the title compound (150 mg) as an oil. Electrospray MS m/z 587 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06218538B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_04 |
|---|
| ORD ID | ord-25ce43649d774d819074daa971a8dfd7 |
|---|
| 출처 메모 | uspto-grants-2001_04 |
|---|