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Triethylamine → 3,4-Dihydro-2-methyl-4-[2-[4-(2-pyrimidinyl)-1-piperazinyl]ethyl]-pyrimido[1,6-a]benzimidazol-1(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(2-Pyrimidinyl)piperazine | HCID 88747 | — |
| 反応物 | 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989845 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3,4-Dihydro-2-methyl-4-[2-[4-(2-pyrimidinyl)-1-piperazinyl]ethyl]-pyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989877 | — |
反応手順
To 60 mL of toluene was added 4.0 g (0.0152 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.0 g (0.033 mol) of 1-(2-pyrimidyl)piperazine, and 4.0 g (0.04 mol) of triethylamine. The reaction mixture was heated at reflux for 2 days and subsequently washed with 2×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. Crystallization from ethyl acetate afforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05063228 |
| 出典データセット | uspto-grants-1991_11 |
| ORD ID | ord-4468c9561fd34ace85f1afffbda719ff |
| 出典メモ | uspto-grants-1991_11 |