1-Methylimidazole → ethyl 1-methyl-1H-imidazole-2-carboxylate
反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.C(#N)C.Cl[C:11]([O:13][CH2:14][CH3:15])=[O:12]>C(N(CC)CC)C>[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:11]([O:13][CH2:14][CH3:15])=[O:12]参加物
5
実験手順
To a solution of N-methylimidazole (5 g, 0.06 mol), acetonitrile (32 mL) and triethylamine (15 mL), cooled to −20° C. was added ethyl chloroformate (13 mL, 0.137 mol), and the mixture allowed to slowly warm to room temperature and stirred for 3.5 hr. The solution was filtered (triethylamine hydrochloride) and concentrated under vacuum. The residue was purified by distillation under reduced pressure (0 Torr, 102° C.) to yield the product as a white solid. Yield (6.26 g, 68%) 1H NMR (DMSO): δ 7.44 (d, 1H, J=2.8 Hz), 7.04 (d, 1H, J=2.8 Hz), 4.26 (q, 2H, J=3.5 Hz), 3.91 (s, 3H), 1.26 (t, 3 h, J=3.5 Hz). 13C (DMSO): 159.3, 129.1, 127.7, 61.0, 36.0, 14.5.
後処理
- filtrationThe solution was filtered (triethylamine hydrochloride)
- concentrationconcentrated under vacuum
- distillationThe residue was purified by distillation under reduced pressure (0 Torr, 102° C.)
出典と根拠
- ORDレコード
- ord-9f7618c45f704826b6686dfd2c837ffc
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08017599B2
反応ノート
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