Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 1,2-Diphenylethyl 1-methylpiperidine-4-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 1,2-Diphenylethanol | HCID 94178 | — |
| 반응물 | 4-Piperidinecarboxylic acid, 1-methyl-, hydrochloride (1:1) | HCID 2760043 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1,2-Diphenylethyl 1-methylpiperidine-4-carboxylate | HCID 70925787 | 37% |
반응 단계
Oxalyl dichloride (141 μl, 1.67 mmol) was added dropwise to a solution of 1-methylpiperidine-4-carboxylic acid hydrochloride (300 mg, 1.67 mmol) in DCM (20 ml) and few drops of DMF (catalytic amount). The reaction was stirred at room temperature for 2 hours. The volatiles were removed under vacuum, and the crude was taken up with pyridine (20 ml). 1,2-Diphenylethanol (331 mg, 1.67 mmol) was added, and the resulting suspension was heated under microwave irradiation at 140° C. for 1 hour. Pyridine was removed under vacuum, and the crude was purified by flash chromatography (DCM/MeOH=97/3 to 94/6) to obtain 1,2-diphenylethyl 1-methylpiperidine-4-carboxylate (200 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08604015B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-b13f5ebe1c75469c810a0348eb917fd9 |
| 출처 메모 | uspto-grants-2013_12 |