Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isobutyryl chloride → N-[2-Chloro-4-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-benzyl]-isobutyramide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isobutyryl chloride | HCID 62325 | — |
| 반응물 | Riboflavin sodium phosphate | HCID 23666409 | — |
| 반응물 | (4-Aminomethyl-3-chloro-phenyl)-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone Hydrochloride | HCID 136346649 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | N-[2-Chloro-4-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-benzyl]-isobutyramide | HCID 135736064 | 40% |
반응 단계
Isobutyryl chloride (46 mg, 0.4 mmol) was added to a solution of (4-aminomethyl-3-chloro-phenyl)-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone hydrochloride from Example E106.2 (161 mg, 0.4 mmol) in dichloromethane (10 ml) and triethylamine (to pH9) at room temperature. The mixture was stirred for 18 h, diluted with EtOAc, washed with saturated NaHCO3 then brine, dried and concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane) to give a white solid identified as the title compound (75 mg, 40%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08202858B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-da4075677e194c8bbf4a635746eef687 |
| 출처 메모 | uspto-grants-2012_06 |