Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Phosphate, Tribasic → {1-[3-(3-Dimethylamino-pyrrolidin-1-yl)-phenyl]-ethyl}-carbamic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | (3R)-(+)-3-(Dimethylamino)pyrrolidine | HCID 2758521 | — |
| 반응물 | (S)-N-Boc-1-(3-bromophenyl)ethylamine | HCID 56971804 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | {1-[3-(3-Dimethylamino-pyrrolidin-1-yl)-phenyl]-ethyl}-carbamic acid tert-butyl ester | HCID 69588726 | 27% |
반응 단계
A mixture of (S )[1-(3-bromo-phenyl)-ethyl]-carbamic acid tert-butyl ester (6 g), (3R)-3-(dimethylamino)-pyrrolidine (4.56 g), Pd2(dba)3 (1.83 g), di-t-butyl-biphenylphosphine (600 mg), K3PO4 (8.48 g) in DME (40 mL) was stirred at reflux for 16 h. The reaction mixture was cooled down to room temperature, diluted with methylene chloride, and filtered. The filtrated was evaporated in vacuo, and the crude product was purified by Flash Chromatography using Biotage eluting with 20% MeOH in ethyl acetate to give the title compound (1.8 g) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07144881B2 |
| 출처 데이터셋 | uspto-grants-2006_12 |
| ORD ID | ord-25c8f9ac53e244bba0ba6badd5929881 |
| 출처 메모 | uspto-grants-2006_12 |