Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfoxide → 1-(4-Methylbenzyl)piperidin-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 1-(4-Methylbenzyl)piperidin-4-ol | HCID 791482 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(4-Methylbenzyl)piperidin-4-one | HCID 11959541 | 81% |
반응 단계
To 2.8 mL (32 mmol) of oxalyl chloride in 75 mL of CH2Cl2 at −78° C. was added 4.6 mL (64 mmol) of DMSO. To this mixture was added 5.3 g (26 mmol) of 1-(4-methylbenzyl)-4-piperidinol 123 in 10 mL of CH2Cl2, and the mixture was stirred 5 min in the cold. The mixture was quenched with 18 mL (129 mmol) of triethylamine and allowed to come to room temperature, and saturated aqueous ammonium chloride was added. The organic phase was washed with water and brine, dried, and evaporated to give 4.27 g (81%) of 1-(4-methylbenzyl)-4-piperidinone (124), which was used as is without further purification. GC/MS showed 100% purity with a molecular ion of 203.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06706740B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-fb7270a74cbc4031b8e83c2f70138da2 |
| 출처 메모 | uspto-grants-2004_03 |