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

HRID 1660453
ノート
印刷プレビュー

反応式

HRID 1660453 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-f74b8be628b14e88afd5ad0cd82ba249
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04308208

反応ノート

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