Morpholine → Morpholine, 4-(2-methoxyethyl)-
反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[CH3:7][O:8][CH2:9][CH2:10]Cl>>[CH3:7][O:8][CH2:9][CH2:10][N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1参加物
3
実験手順
In an autoclave of 100 mL, morpholine (45.0 g, 517 mmol) was made reacted with chloroethyl methyl ether (25.0 g, 265 mmol) at 130 deg C. for 48 hours. Solid salt that was formed was removed by filtration, and residue (filtrate) was subjected to reduced-pressure distillation by using a Vigreux column of 25 cm. Then 1H-NMR measurement of obtained amine is performed, and it was confirmed that chemical shifts, δ (ppm), are 3.53-3.55(m, 4H), 3.33-3.35(m, 2H), 3.17(s, 3H), and 2.36-2.32 (m, 6H), and that N-2-methoxyethylmorpholine was synthesized.
後処理
- customSolid salt that was formed
- customwas removed by filtration, and residue (filtrate)
- distillationwas subjected to reduced-pressure distillation
出典と根拠
- ORDレコード
- ord-569b4e245c044095ae2153b5d5a9beb1
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09379413B2
反応ノート
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