Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trimethylaluminum → HCID 178489759, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trimethylaluminum | HCID 16682925 | — |
| 반응물 | Ethyl ether methylene chloride | HCID 21881112 | — |
| 반응물 | Ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoate | HCID 66589916 | — |
| 반응물 | HCID 178489815 | HCID 178489815 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 178489759 | HCID 178489759 | 33.7% |
반응 단계
4-(4-cyclopropyl-1,4-diazepan-1-yl)-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]benzamide was prepared using the same procedure as for Example 159, but starting from ethyl 4-(4-cyclopropyl-1,4-diazepan-1-yl)benzoate (0.288 g, 1 mmol, 5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-amine (0.247 g, 1 mmol) and a 2M solution of trimethylaluminium (1.250 mL, 2.50 mmol) in toluene. The crude product was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford a gum which solidified on trituration with DCM/Ether to afford the title compound (0.165 g, 33.7%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08604022B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-713099bb3ca4476bb6bc5dad14f55bba |
| 출처 메모 | uspto-grants-2013_12 |