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

HRID 359082
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HRID 359082 반응식
[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
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참가 물질

7

반응물 4

HCID 313Hydrochloric Acid2회HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 15086593HCID 15086593, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol
용매
3회
HCID 962Water용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d8de91afe1943239e39dfc918035043
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04999378

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