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

HRID 1485435
ノート
印刷プレビュー

反応式

HRID 1485435 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-7ecca4a3beff4a488eef176959f172b2
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09422292B2

反応ノート

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