Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfoxide → 1-N-Cbz-3-pyrrolidinone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | Benzyl 3-hydroxypyrrolidine-1-carboxylate | HCID 560953 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-N-Cbz-3-pyrrolidinone | HCID 561203 | — |
반응 단계
150 ml of oxalic acid chloride was added to 2 liters of dichloromethylene. 245 ml of dimethylsulfoxide was gradually added at -70° to -50° C. in a stream of argon. 70.67 g of N-(N-(benzyloxycarbonyl)-3-pyrrolidinol dissolved in dichloromethylene was dropped. After gradual dropping of 720 ml of triethylamine, the mixture was raised to room temperature. After completion of the reaction, the reaction solution was poured into water and extracted with dichloromethylene, followed by removal of the solvent by distillation under reduced pressure. The residue was purified by column chromatography (eluting solvent: hexane-ethyl acetate), thereby obtaining 66.55 g of the intended compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468740 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-ea7c1b7701d14646b5be5ae07b542132 |
| 출처 메모 | uspto-grants-1995_11 |