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Ethyl Acetate → HCID 19089105、化合物

HRID 1463977
ノート
印刷プレビュー

反応式

HRID 1463977 の反応式
[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH2:5][NH:6][NH2:7])[CH3:2].CO[C:13](=[CH2:16])[C:14]#[N:15].C(OCC)(=O)C>O>[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH2:5][N:6]1[C:14]([NH2:15])=[CH:13][CH:16]=[N:7]1)[CH3:2]
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 322952(2,2-Diethoxyethyl)hydrazineHCID 132442492-Methoxyprop-2-enenitrile

生成物 1

HCID 19089105HCID 19089105、化合物収率 19.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of hydrazinoacetaldehyde diethyl acetal (21 g) and methoxyacrylonitrile (11.8 g) in water (150 ml) was refluxed for 2 days. After the reaction mixture was cooled, to the mixture was added a mixture of water and ethyl acetate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was evaporated and the residue was subjected to column chromatography on silica gel using ethyl acetate as an eluent. Fractions containing the object compound were combined and evaporated to give 1-(2,2-diethoxyethyl)-5-aminopyrazole (5.45 g).

後処理

  1. temperaturewas refluxed for 2 days
  2. temperatureAfter the reaction mixture was cooled, to the mixture
  3. additionwas added
  4. washThe separated organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. additionFractions containing the object compound
  8. customevaporated

出典と根拠

ORDレコード
ord-18a4391a669a48c38274b7f29de18659
出典データセット
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05302712

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート