Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → (S)-benzyl 3-carbamoyl-3-methylpyrrolidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 반응물 | (S)-1-((benzyloxy)carbonyl)-3-methylpyrrolidine-3-carboxylic acid | HCID 76853756 | — |
| 반응물 | Water ammonium hydroxide | HCID 86589665 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | (S)-benzyl 3-carbamoyl-3-methylpyrrolidine-1-carboxylate | HCID 86707398 | 95.6% |
반응 단계
To a mixture of (S)-1-(benzyloxycarbonyl)-3-methylpyrrolidine-3-carboxylic acid (32.87 g, 124.8 mmol), Boc2O (29.97 g, 137.3 mmol) in ethyl acetate (200 mL) was added pyridine (12.62 mL, 156.1 mmol) and the reaction mixture was stirred at ambient temperature for 3 hours. A solution of 28-30% w/w NH4OH/water (21.79 mL, 162.3 mmol) was added. The reaction was stirred at ambient temperature for 5 hours. Water (50 mL) was added. The organic layer was separated, washed with 1N HCl (50 mL) and brine, dried and concentrated under reduced pressure to give (S)-benzyl 3-carbamoyl-3-methylpyrrolidine-1-carboxylate (31.30 g, 119.3 mmol, 95.6% yield) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08889704B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-a151995ce2644fc89a3d897ae133fc4c |
| 출처 메모 | uspto-grants-2014_11 |