Ethanol → 4-Chloro-5-(cyclopentyloxy)-2-fluorobenzenamine

HRID 275098

반응식

HRID 275098 반응식
[OH-].[Na+].C(O)C.[F:6][C:7]1[CH:12]=[C:11]([Cl:13])[C:10]([O:14][CH:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:9][C:8]=1[NH:20]C(=O)OC>O>[F:6][C:7]1[CH:12]=[C:11]([Cl:13])[C:10]([O:14][CH:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:9][C:8]=1[NH2:20]

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 15766845methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate

생성물 1

HCID 152793894-Chloro-5-(cyclopentyloxy)-2-fluorobenzenamine수율 100%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2N sodium hydroxide aqueous solution (3.5 ml) was added to an ethanol solution (1.5 ml) of methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate (1.507 g, 5.24 mmol), and the mixture was heated under reflux for 2 hours. After reaction, the reaction liquid was cooled to room temperature, water was added thereto, and this was extracted with ethyl acetate (20 ml×2). The organic layer was washed with water and saturated brine and then dried over anhydrous magnesium sulfate. The drying agent was taken out by filtration, and the solvent was removed by distillation under reduced pressure, to obtain 2-fluoro-4-chloro-5-cyclopentyloxyaniline (1.20 g, 5.22 mmol). Yield: ~100%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customAfter reaction
  4. customthe reaction liquid
  5. extractionthis was extracted with ethyl acetate (20 ml×2)
  6. washThe organic layer was washed with water and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationThe drying agent was taken out by filtration
  9. customthe solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-76c0d1ed09184dc19b11d51e7b86c166
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391807

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