Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium hydride → diethyl {((1,1-dimethylethoxycarbonyl)-1H-benzimidazole-4-yl)methyl}(dipropylamino)-propanedioate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium hydride | HCID 82127 | — |
| 반응물 | tert-Butyl 4-(bromomethyl)-1H-benzo[d]imidazole-1-carboxylate | HCID 15744964 | — |
| 반응물 | Diethyl (dipropylamino)propanedioate | HCID 15744966 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | diethyl {((1,1-dimethylethoxycarbonyl)-1H-benzimidazole-4-yl)methyl}(dipropylamino)-propanedioate | HCID 15744967 | 80.7% |
반응 단계
Potassium hydride (3.3 g of 40% oil suspension, washed with ether to remove oil, 0.03 mol) was added to a stirred solution of diethyl (dipropylamino)-malonate (10.2 g, 0.039 mol) in dry THF (100 mL). After 5 minutes, t-butyl 4-(bromomethyl) -1H-benzimidazole-1-carboxylate (6.22 g, 0.02 mol) was added and the solution was refluxed for 6 hours. The solvent was removed under reduced pressure and the residual oil was partitioned between ethyl acetate and water. After evaporation of the ethyl acetate, the crude product was chromatographed on silica gel using ethyl acetate:hexane as the eluant to give 7.9 g of diethyl {((1,1 -dimethylethoxycarbonyl)-1H-benzimidazole-4-yl)methyl}(dipropyl amino)-propanedioate as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05436240 |
| 출처 데이터셋 | uspto-grants-1995_07 |
| ORD ID | ord-02c10acca5c44d4182e4e0f418745082 |
| 출처 메모 | uspto-grants-1995_07 |