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Ammonium Chloride → Methyl 3-(2-amino-4-fluorophenylamino)-2-methylpropanoate

HRID 1485435
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HRID 1485435 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][CH:10]([CH3:15])[C:11]([O:13][CH3:14])=[O:12])=[C:4]([N+:16]([O-])=O)[CH:3]=1.[Cl-].[NH4+]>C(O)C.[Zn]>[NH2:16][C:4]1[CH:3]=[C:2]([F:1])[CH:7]=[CH:6][C:5]=1[NH:8][CH2:9][CH:10]([CH3:15])[C:11]([O:13][CH3:14])=[O:12]
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참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 70978244Methyl 3-(4-fluoro-2-nitrophenylamino)-2-methylpropanoate

생성물 1

HCID 86718504Methyl 3-(2-amino-4-fluorophenylamino)-2-methylpropanoate수율 81%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 702Ethanol용매

실험 절차

To a solution of methyl 3-(4-fluoro-2-nitrophenylamino)-2-methylpropanoate (14.0 g, 54.6 mmol) in ethanol (250 mL) were added zinc powder (14.2 g, 218 mmol) and saturated ammonium chloride (28.4 mL) at 0° C. Once addition was completed, the reaction mixture was stirred at reflux for 1 hour. Then the mixture was cooled to room temperature, filtered, and washed with ethanol (200 mL). The organic phase was concentrated in vacuo, dissolved in water (250 mL), and extracted with ethyl acetate (200 mL*3). The combined organic layers was separated, dried over anhydrous sodium sulfate, and concentrated to give a residue. The residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=2:1) to afford methyl 3-(2-amino-4-fluorophenylamino)-2-methylpropanoate as a black solid (10.0 g, 81%).

후처리

  1. additionOnce addition
  2. temperatureat reflux for 1 hour
  3. filtrationfiltered
  4. washwashed with ethanol (200 mL)
  5. concentrationThe organic phase was concentrated in vacuo
  6. dissolutiondissolved in water (250 mL)
  7. extractionextracted with ethyl acetate (200 mL*3)
  8. customThe combined organic layers was separated
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationconcentrated
  11. customto give a residue
  12. customThe residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-7ecca4a3beff4a488eef176959f172b2
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422292B2

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