Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sec-Butylamine → 4-[(S)-3-(tert-butoxycarbonylamino)pyrrolidin-1-yl]-2-sec-butylamino-3-chloro-5-fluorobenzoic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sec-Butylamine | HCID 24874 | — |
| 반응물 | 4-[(S)-3-tert-Butoxycarbonylaminopyrrolidin-1-yl]-3-chloro-2,5-difluorobenzoic acid ethyl ester | HCID 58681894 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-[(S)-3-(tert-butoxycarbonylamino)pyrrolidin-1-yl]-2-sec-butylamino-3-chloro-5-fluorobenzoic acid ethyl ester | HCID 86607130 | 167.5% |
반응 단계
4-[(S)-3-(tert-Butoxycarbonylamino)pyrrolidin-1-yl]-3-chloro-2,5-difluorobenzoic acid ethyl ester (Example 2c, 1.95 g, 4.81 mmol), sec-butylamine (30 mL, 296 mmol), and dimethyl sulfoxide (20 mL) are heated in a sealed glass tube at 110° C. for 24 hours. The reaction mixture is evaporated, and purification by column chromatography (1:8, ethyl acetate/hexanes) provides the title compound as a yellow syrup (3.69 g). MS EI: m/z 458 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094780B1 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-c9ad7ba81a844b13b2fa7d7f9fd4ed34 |
| 출처 메모 | uspto-grants-2006_08 |