Bis(2-chloroethyl) ether → 4-(3-Methoxyphenyl)morpholine

HRID 884429

반응식

HRID 884429 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.C(N(C(C)C)CC)(C)C>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

참가 물질

5

반응물 3

HCID 8115Bis(2-chloroethyl) etherHCID 108243-MethoxyanilineHCID 81531Diisopropylethylamine

생성물 1

HCID 99643354-(3-Methoxyphenyl)morpholine수율 77.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of m-anisidine (11.2 mL, 0.1 mol), chloroethyl ether (11.7 mL, 0.1 mol), and diisopropylethylamine (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

  1. temperatureat reflux for 72 h
  2. customThe precipitate was removed by filtration
  3. washwashed with toluene (100 mL)
  4. concentrationThe combined toluene solutions were concentrated in vacuo
  5. distillationpurified by distillation (120-130° C., 0.2 Torr)

출처 및 근거

ORD 기록
ord-734dd9a18be44d608faa48acba7c156f
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242115B2

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