Triethylamine → N-ethoxalyl-N-(2-phthalimido)ethyl-4-(2,2,3,3-tetrafluoropropoxy)aniline

HRID 482053ノート

反応式

HRID 482053 の反応式
[C:1]1(=[O:28])[N:5]([CH2:6][CH2:7][NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]([F:22])([F:21])[CH:18]([F:20])[F:19])=[CH:11][CH:10]=2)[C:4](=[O:23])[C:3]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:2]12.C(N(CC)CC)C.Cl[C:37](=[O:43])[C:38]([O:40][CH2:41][CH3:42])=[O:39]>ClCCl>[C:37]([N:8]([CH2:7][CH2:6][N:5]1[C:4](=[O:23])[C:3]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:2]2[C:1]1=[O:28])[C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:16][C:17]([F:22])([F:21])[CH:18]([F:19])[F:20])=[CH:13][CH:14]=1)([C:38]([O:40][CH2:41][CH3:42])=[O:39])=[O:43]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 19065098N-(2-phthalimido)ethyl-4-(2,2,3,3-tetrafluoropropoxy)aniline

生成物 1

HCID 86749721N-ethoxalyl-N-(2-phthalimido)ethyl-4-(2,2,3,3-tetrafluoropropoxy)aniline

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-40 °C

実験手順

To the mixture of the obtained N-(2-phthalimido)ethyl-4-(2,2,3,3-tetrafluoropropoxy)aniline (3.2 g), triethylamine (1.2 ml) and dichloromethane (60 ml), was added dropwise a solution of ethyl chloroglyoxylate (0.9 ml) in dichloromethane (10 ml) at -65° C. The reaction solution was stirred for 1 hour at -40° C., and then ice-water (50 ml) was added thereto to fractionate. The dichloromethane layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give N-ethoxalyl-N-(2-phthalimido)ethyl-4-(2,2,3,3-tetrafluoropropoxy)aniline (3.1 g) as colorless powdery crystals.

後処理

  1. washThe dichloromethane layer was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure
  4. customThe residue was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-5a0f0de434c74bf3920ee54530e32bac
出典データセット
uspto-grants-1998_08
特許番号
US05792780

反応ノート

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