Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Pyridine-2-carboxylic acid 4-(pyrrolidine-1-carbonyloxymethyl)-cyclohexyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Pyridine-2-carbonyl chloride | HCID 135034 | — |
| 반응물 | Pyrrolidine-1-carboxylic acid 4-hydroxycyclohexylmethyl ester | HCID 66837799 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Pyridine-2-carboxylic acid 4-(pyrrolidine-1-carbonyloxymethyl)-cyclohexyl ester | HCID 56952073 | 70.1% |
반응 단계
To a solution of pyrrolidine-1-carboxylic acid 4-hydroxy-cyclohexylmethyl ester (1 mmol) in methylene chloride (5 mL) were added picolinoyl chloride (1.1 mmol) and triethylamine (1.5 mmol) and the resulting mixture was stirred for 16 hours at room temperature. The reaction mixture was diluted with water, followed by few times of extraction with methylene chloride. The combined organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, ethyl acetate), thereby completing the preparation of a target compound (233 mg, 70% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822463B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-cbcbb27e30584e42ab30cd8da7dcaf04 |
| 출처 메모 | uspto-grants-2014_09 |