関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | N-Methylaniline | HCID 7515 | — |
| 反応物 | 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989845 | — |
| 生成物 | 3,4-Dihydro-2-methyl-4-[2-(methylphenylamino)ethyl]pyrimido[1.6-a]benzimidazol-1(2H)-one | HCID 19989884 | — |
反応手順
To 15 mL of N-methylaniline was added 3.5 g (0.0133 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one. The reaction mixture was heated to 90° C. (oil bath) for 2 days, and the excess N-methylaniline removed in vacuo at 80° C., 0.5 mm Hg. The residue was dissolved in 100 mL of CH2Cl2, washed with 2×100 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was subjected to high vacuum (0.5 mm, Hg) at 85° C. for 2 hr, and then crystallized from iso-octane/toluene to give 2.3 g (52%) of analytically pure crystals, mp 130°-31° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05063228 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-c78e2a38ff4646a4a82c085bb73e74cf |
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| 出典メモ | uspto-grants-1991_11 |
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