Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanol → HCID 58120261, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Benzene, 2,4-dichloro-1-fluoro- | HCID 123112 | — |
| 반응물 | (S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic Acid t-Butyl Ester | HCID 66858889 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 58120261 | HCID 58120261 | — |
반응 단계
(S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic acid t-butyl ester (25.0 mg, 96.4 mmol) was dissolved in DMF (200 μL). NaH (2776 μg, 115.7 mmol) was added and the mixture was stirred at room temperature for 15 minutes. 2,4-Dichloro-1-fluorobenzene (22.6 μL, 192.8 μmol) was added and the mixture was stirred at 70° C. for 3 hours. The mixture was concentrated then dissolved in 1.2M HCl in EtOH (1.0 mL, 1.2 mmol) and stirred overnight. The product was concentrated and purified by preparative HPLC (10-40%, 60 min, BDS) to yield the title compound as a mono-TFA salt oil (24.4 mg, 100% purity). MS m/z: [M+H]+ calcd for C14H19Cl2NO2, 304.08; found 304.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08273786B2 |
| 출처 데이터셋 | uspto-grants-2012_09 |
| ORD ID | ord-e70328b0129d4c18a986025936216f11 |
| 출처 메모 | uspto-grants-2012_09 |