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

HRID 349680

反応式

HRID 349680 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>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

反応物 2

HCID 8115Bis(2-chloroethyl) etherHCID 108243-Methoxyaniline

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 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

  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-7d679226bb9f4cc49a0bf6f5f638a0ef
出典データセット
uspto-grants-2007_02
特許番号
US07179912B2

関連ノート

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