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

HRID 884429

反応式

HRID 884429 の反応式
[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.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

参加物

5

反応物 3

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

生成物 1

HCID 99643354-(3-Methoxyphenyl)morpholine収率 77.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-734dd9a18be44d608faa48acba7c156f
出典データセット
uspto-grants-2012_08
特許番号
US08242115B2

関連ノート

読み込み中…