Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → (S)-3-[(S)-1-(2,3-Dichlorophenoxy)-3-methylbutyl]pyrrolidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Benzene, 1,2-dichloro-3-fluoro- | HCID 119011 | — |
| 반응물 | (S)-tert-Butyl 3-((S)-1-hydroxy-3-methylbutyl)pyrrolidine-1-carboxylate | HCID 57347268 | — |
| 생성물 | (S)-3-[(S)-1-(2,3-Dichlorophenoxy)-3-methylbutyl]pyrrolidine | HCID 58104615 | — |
반응 단계
(S)-3-((S)-1-Hydroxy-3-methylbutyl)pyrrolidine-1-carboxylic acid t-butyl ester (50 mg, 0.2 mmol) was dissolved in DMF (940 μL, 12 mmol). Sodium hydride (5.6 mg, 233 μmmol) was then slowly added, and the mixture was stirred at room temperature for 15 minutes. 1,2-Dichloro-3-fluoro-benzene (64.1 mg, 388 μmmol) was added. The mixture was stirred at 70° C. for 3 hours, then concentrated under vacuum. 1.2M HCl in EtOH (1.1 mL, 1.3 mmol) was added, and the mixture was stirred overnight. The product was concentrated and purified by preparative HPLC to yield the title compound as a mono-TFA salt (37.4 mg, 100% purity). MS m/z: [M+H]+ calcd for C15H21Cl2NO, 302.10; found 302.2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07994209B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-f6b683a4465c472dbb74fd8f4fb65980 |
| 출처 메모 | uspto-grants-2011_08 |