Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → HCID 59347881, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 2-Chloro-3-(trifluoromethyl)benzoic acid | HCID 2736677 | — |
| 반응물 | [2-Methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine | HCID 59347786 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 59347881 | HCID 59347881 | — |
반응 단계
A mixture of [2-methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine D26 (0.150 g; 0.647 mmol), 2-chloro-3-(trifluoromethyl)benzoic acid (0.174 g; 0.775 mmol), EDC (0.149 g; 0.777 mmol) and HOBt (0.020 g; 0.148 mmol) in DCM (4 ml) was shaken at room temperature for 66 hours. Saturated sodium hydrogen carbonate (8 ml) was added and shaking continued for 0.5 hours. The organic layer was passed through a phase separation cartridge and applied to a 2 g SCX column. The column was washed with DCM and methanol and the product eluted with 1M ammonia in methanol. The crude product was purified by chromatography on silica gel (20 g) eluting with 0-100% ethyl acetate in pentane gradient to afford the title compound as two pairs of enantiomers.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745642B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-d442d140b910474784016bfda8a268a9 |
| 출처 메모 | uspto-grants-2010_06 |