Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Phenylpiperazine → 3,4-Dihydro-2-methyl-4-[2-(4-phenyl-1-piperazinyl)ethyl]pyrimido[1,6-a]benzimidazol-1(2H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Phenylpiperazine | HCID 7096 | — |
| 반응물 | 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989845 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3,4-Dihydro-2-methyl-4-[2-(4-phenyl-1-piperazinyl)ethyl]pyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989850 | — |
반응 단계
To 4.0 g (0.015 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one in 35 mL of toluene was added 6.5 g (0.04 mol) of N-phenylpiperazine. The reaction mixture was heated to reflux for 2 days. The entire reaction mixture was washed with 3×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was subjected to preparative HPLC using acetone as the eluent and silica gel as the stationary phase. Like fractions were combined, concentrated and the residue crystallized from isopropyl alcohol to give 3.7 g (64%) of analytically pure, crystalline material, mp 143.5°-145.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05063228 |
| 출처 데이터셋 | uspto-grants-1991_11 |
| ORD ID | ord-ada81d8a687f4554b66e8723a64677dc |
| 출처 메모 | uspto-grants-1991_11 |