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Hydrazine hydrate (1:1) → Methyl alpha-methylthio-alpha-(3-chloro-4-aminophenyl)propionate

HRID 1733630
ノート
印刷プレビュー

反応式

HRID 1733630 の反応式
[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][C:12]([N:15]2C(=O)C3=CC=CC=C3C2=O)=[C:11]([Cl:26])[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5].O.NN>CO>[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:26])[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 12819454Methyl alpha-methylthio-alpha-(3-chloro-4-phthalimidophenyl)propionate

生成物 1

HCID 12917666Methyl alpha-methylthio-alpha-(3-chloro-4-aminophenyl)propionate収率 92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl α-methylthio-α-(3-chloro-4-phthalimidophenyl)propionate was suspended in 7 ml of methanol, and 97 mg of hydrazine hydrate was added. The mixture was stirred at room temperature, and then heated under reflux for 1 hour. The mixture was concentrated under reduced pressure, and an aqueous solution of ammonium chloride and methylene chloride were added. The organic layer was separated, and dried over anhydrous sodium sulfate. Concentration under reduced pressure yielded 231 mg of methyl α-methylthio-α-(3-chloro-4-aminophenyl)propionate as a pale yellow oil. Yield 92%.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionan aqueous solution of ammonium chloride and methylene chloride were added
  5. customThe organic layer was separated
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationConcentration under reduced pressure

出典と根拠

ORDレコード
ord-c19e05afcdd54fbe9788054086601665
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04242519

反応ノート

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