Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyrrolidine → 1-[(4-Bromophenoxy)acetyl]pyrrolidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyrrolidine | HCID 31268 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | p-Bromophenoxyacetic acid | HCID 74657 | — |
| 촉매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-[(4-Bromophenoxy)acetyl]pyrrolidine | HCID 787679 | — |
반응 단계
Oxalyl chloride (0.5 mL, 5.9 mmol) was added to a suspension of (4-bromophenoxy)acetic acid (0.462 g, 2.0 mmol) in methylene chloride (10 mL) and 2 drops of N,N-dimethylformamide. The mixture was stirred at RT for 2 h. The solvent was evaporated under reduced pressure. The residue was diluted with methylene chloride (10 mL), cooled with ice-water bath, and 1M of sodium hydroxide aqueous solution (3.0 mL) was added. To the mixture was added pyrrolidine (167 μL, 2.0 mmol). The mixture was stirred and allowed to warm to RT. The organic layer was separated, washed with water and brine, dried over Na2SO4, filtered, and concentrated. The residue was directly used in next step without further purification (550 mg, 96.7%). LCMS: (M+H)=286.0/284.0
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07767675B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-746b17a2070148b2ad2b77f13ddfa069 |
| 출처 메모 | uspto-grants-2010_08 |