Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Methyl triflate | HCID 9526 | — |
| 반응물 | 3-Cyano-4-dimethylamino-benzoic acid methyl ester | HCID 59847657 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate | HCID 86621519 | 69% |
반응 단계
To a stirred solution of 6.16 g (30.2 mmol) 3 and 110 ml dichloromethane were added 50.0 g (302 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was stirred over night and diethylether was added. After evaporation of one third of the solvent volume the desired compound precipitates and the rest of the solvent were decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water—gradient 1:99 to 80:20). The desired compound 4 was obtained in 69% yield (20.8 mmol, 7.68 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08557776B2 |
| 출처 데이터셋 | uspto-grants-2013_10 |
| ORD ID | ord-14848f56a14a460f8cd5383286b8ca90 |
| 출처 메모 | uspto-grants-2013_10 |