Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,1'-Carbonyldiimidazole → NGB 2904 hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 9H-fluorene-2-carboxylic acid | HCID 348591 | — |
| 반응물 | 1-Piperazinebutanamine, 4-(2,3-dichlorophenyl)- | HCID 11098669 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | NGB 2904 hydrochloride | HCID 19366304 | 139.4% |
반응 단계
A mixture of 9H-fluorene-2-carboxylic acid (100 mg, 0.48 mmol) and 1.1'-carbonyldiimidazole (80 mg, 0.5 mmol) in 10 mL of anhydrous tetrahydrofuran was stirred for 8 hours. A solution of 4-[4-(2,3-dichlorophenyl)-1-piperazinyl]-1-aminobutane (150 mg, 0.5 mmol) in 1 mL of tetrahydrofuran was added and the resulting mixture was stirred for 30 minutes. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with aqueous Na2CO3 solution, dried (Na2SO4) and concentrated in vacuo to give the title compound (185 mg, 78%). Hydrochloride salt was prepared by treating the free base with a solution of hydrogen chloride in ethyl acetate (mp 262-4° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06015900 |
| 출처 데이터셋 | uspto-grants-2000_01 |
| ORD ID | ord-2492c9d164984b47b86e64cff738f390 |
| 출처 메모 | uspto-grants-2000_01 |