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Hydrochloric Acid → 4-[2-[N-(4-Chlorophenyl)amino]ethoxy]benzoic acid hydrochloride

HRID 359082
ノート
印刷プレビュー

反応式

HRID 359082 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][CH2:10][O:11][C:12]2[CH:21]=[CH:20][C:15]([C:16]([O:18]C)=[O:17])=[CH:14][CH:13]=2)=[CH:4][CH:3]=1.[OH-].[Na+].Cl.CCOCC>CO.O>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][C:15]([C:16]([OH:18])=[O:17])=[CH:20][CH:21]=2)=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 15086593HCID 15086593、化合物

生成物 1

HCID 678278944-[2-[N-(4-Chlorophenyl)amino]ethoxy]benzoic acid hydrochloride収率 144.4%

試薬・触媒・溶媒 2

HCID 887Methanol
溶媒
3 回
HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

Methyl 4-[2-[N-(4-chlorophenyl)amino]ethoxy]benzoate (0.4 g) was suspended in methanol (20 ml), and thereto a solution of sodium hydroxide (0.16 g) in water (5 ml) was added, and the mixture was heated with stirring at 60° C. for 3 hours. The reaction mixture was cooled, and neutralized with hydrochloric acid and concentrated under reduced pressure. After adding water thereto, the resulting residue was crushed, then, collected by filtration to give crude crystal. An equivalent amount of hydrochloric acid was added to the crude crystal in methanol, and the mixture was dried under reduced pressure to give a salt. The salt was suspended in a mixed solvent of methanol and ether, and collected by filtration to give the desired product (0.31 g). mp. 190°-193° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure
  4. additionAfter adding water
  5. customthe resulting residue was crushed
  6. filtrationcollected by filtration
  7. customto give crude crystal
  8. customthe mixture was dried under reduced pressure
  9. customto give a salt
  10. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-6d8de91afe1943239e39dfc918035043
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04999378

反応ノート

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