Hydrazine hydrate (1:1) → HCID 55285667、化合物

HRID 1943931ノート

反応式

HRID 1943931 の反応式
[CH:1]([NH:4]/[C:5](/SC)=[CH:6]/[C:7]#[N:8])([CH3:3])[CH3:2].O.[NH2:12][NH2:13]>CCO>[CH:1]([NH:4][C:5]1[CH:6]=[C:7]([NH2:8])[NH:13][N:12]=1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86652503(2Z)-3-[(1-Methylethyl)amino]-3-(methylthio)-2-propenenitrile

生成物 1

HCID 55285667HCID 55285667、化合物収率 62.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of (Z)-3-(isopropylamino)-3-(methylthio)acrylonitrile (0.413 g, 2.64 mmol) and hydrazine monohydrate (0.38 mL, 7.93 mmol) in EtOH (6 mL) was heated to reflux for 16 hours. After cooling to room temperature, the reaction mixture was concentrated. The residue was purified by column chromatography, eluting with ethyl acetate, DCM/MeOH (9:1) to give N3-isopropyl-1H-pyrazole-3,5-diamine (0.231 g, 62% over 2 steps) as an oil.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours
  3. concentrationthe reaction mixture was concentrated
  4. customThe residue was purified by column chromatography
  5. washeluting with ethyl acetate, DCM/MeOH (9:1)

出典と根拠

ORDレコード
ord-1aa0d19f5a26406592838b4bfdc8bdfc
出典データセット
uspto-grants-2013_03
特許番号
US08394795B2

反応ノート

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