Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → tert-butyl 3-{[6-(4-fluorophenyl)-2,3-dihydropyrido[3,2-f][1,4]oxazepin-4(5H)-yl]carbonyl}benzylcarbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 3-(((tert-Butoxycarbonyl)amino)methyl)benzoic acid | HCID 2755929 | — |
| 반응물 | 6-(4-Fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine | HCID 69078154 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | tert-butyl 3-{[6-(4-fluorophenyl)-2,3-dihydropyrido[3,2-f][1,4]oxazepin-4(5H)-yl]carbonyl}benzylcarbamate | HCID 67180248 | 89.8% |
반응 단계
To a solution of 6-(4-fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.20 g) obtained in Reference Example 13C, 1-hydroxy-1H-benzotriazole (0.15 g), triethylamine (0.083 g) and 3-(tert-butoxycarbonylaminomethyl)benzoic acid (0.205 g) in acetonitrile (10 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.314 g), and the mixture was stirred at room temperature for 20 hrs. Ethyl acetate was added to the reaction mixture, and the mixture was washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography to give the title compound (0.35 g) as a colorless amorphous powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07625887B2 |
| 출처 데이터셋 | uspto-grants-2009_12 |
| ORD ID | ord-43c476ba5ce64a4b9cf6588523737150 |
| 출처 메모 | uspto-grants-2009_12 |