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Ethyl Acetate → 1-Methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate

HRID 379075
ノート
印刷プレビュー

反応式

HRID 379075 の反応式
[O:1]([C:8]1[CH:9]=[C:10]([NH:14][NH2:15])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OCC)(=O)C.Cl[C:23]([O:25][CH:26]([CH2:28][CH3:29])[CH3:27])=[O:24]>N1C=CC=CC=1>[O:1]([C:8]1[CH:9]=[C:10]([NH:14][NH:15][C:23]([O:25][CH:26]([CH3:27])[CH2:28][CH3:29])=[O:24])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 3

HCID 8857Ethyl AcetateHCID 11829505sec-Butyl chloroformateHCID 21697795(3-Phenoxyphenyl)hydrazine

生成物 1

HCID 216977971-Methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To 3.0 g of 3-phenoxyphenyl hydrazine, 100 ml of ethyl acetate and 2.5 ml of pyridine were added and the resultant solution was then stirred at room temperature for 30 minutes. Then, 2.5 ml of sec-butyl chloro-formate was added dropwise to the solution and stirred for 1 hour at room temperature. The solution was then washed twice, each time with 100 ml of water. After each wash, the aqueous fraction was removed from the organic (ethyl acetate) fraction. The resulting ethyl acetate fraction was then dried over anhydrous sodium sulfate, evaporated under reduced pressure, and then purified by column chromatography on silica gel, to produce 1.5 g of 1-methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate as an oil.

後処理

  1. washThe solution was then washed twice
  2. customAfter each wash, the aqueous fraction was removed from the organic (ethyl acetate) fraction
  3. dry with materialThe resulting ethyl acetate fraction was then dried over anhydrous sodium sulfate
  4. customevaporated under reduced pressure
  5. custompurified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-3091d23f772d4576837ca4b5f6f655b4
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06297275B1

反応ノート

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