Bis(2-chloroethyl) ether → 4-(3-Methoxyphenyl)morpholine
반응식
[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]=1참가 물질
4
실험 절차
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%).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-7d679226bb9f4cc49a0bf6f5f638a0ef
- 출처 데이터셋
- uspto-grants-2007_02
- 특허 번호
- US07179912B2
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