関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 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-(4-morpholinyl)ethyl]pyrimido[1.6-a]benzimidazol-1(2H)-one | HCID 19989856 | — |
反応手順
To 20 mL of morpholine 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 in 60° C. for 24 hrs. The excess morpholine was removed by rotary evaporation and finally by high vacuum (0.5 mm Hg ~60° C.). The residue was dissolved in ~100 mL of CH2Cl2 washed with 3×50 ml of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was crystallized from isopropyl ether to give 2.7 g (65%) of analytically pure crystals, mp 111°-12° 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-7703edcb36b048dc9afb2e9593ef9a78 |
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| 出典メモ | uspto-grants-1991_11 |
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