Bis(2-chloroethyl) ether → 4-(3-Methoxyphenyl)morpholine
反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([NH2:9])[CH:4]=1.Cl[CH2:11][CH2:12][O:13][CH2:14][CH2:15]Cl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[CH:6]=[CH:7][CH:8]=1参加物
4
実験手順
A solution of m-anisidine (11.2 mL, 0.1 mol), chloroethyl ether (11.7 mL, 0.1 mol), and diisopropylethylarine (35 mL, 0.2 mol) in toluene (100 mL) was stirred at reflux for 72 h. The precipitate was removed by filtration and washed with toluene (100 mL). The combined toluene solutions were concentrated in vacuo and purified by distillation (120–130° C., 0.2 Torr) to afford the intermediate 4-(3-methoxyphenyl)-morpholine (14.9 g, 77%).
後処理
- temperatureat reflux for 72 h
- customThe precipitate was removed by filtration
- washwashed with toluene (100 mL)
- concentrationThe combined toluene solutions were concentrated in vacuo
- distillationpurified by distillation (120–130° C., 0.2 Torr)
出典と根拠
- ORDレコード
- ord-7d679226bb9f4cc49a0bf6f5f638a0ef
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07179912B2
反応ノート
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