Hydrazine hydrate (1:1) → 4-(4-Cyclobutylpiperazin-1-yl)-6-hydrazinopyrimidine

HRID 2039475ノート

反応式

HRID 2039475 の反応式
O.[NH2:2][NH2:3].Cl[C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1>C(O)C>[CH:17]1([N:14]2[CH2:15][CH2:16][N:11]([C:9]3[CH:10]=[C:5]([NH:2][NH2:3])[N:6]=[CH:7][N:8]=3)[CH2:12][CH2:13]2)[CH2:20][CH2:19][CH2:18]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 579250694-Chloro-6-(4-cyclobutylpiperazin-1-yl)pyrimidine

生成物 1

HCID 462211044-(4-Cyclobutylpiperazin-1-yl)-6-hydrazinopyrimidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

At RT, 4.4 ml (4.5 g, 89.7 mmol) of hydrazine hydrate are added dropwise with stirring to a solution of 1.9 g (7.5 mmol) of 4-chloro-6-(4-cyclobutylpiperazin-1-yl)pyrimidine in 28 ml of ethanol. The reaction solution is stirred at 80° C. for 16 h. For work-up, the mixture is concentrated under reduced pressure, the residue is triturated repeatedly with diethyl ether, and the precipitated solid is filtered off and dried under reduced pressure. The residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2). Yield: 1.5 g (80% of theory)

後処理

  1. concentrationFor work-up, the mixture is concentrated under reduced pressure
  2. customthe residue is triturated repeatedly with diethyl ether
  3. filtrationthe precipitated solid is filtered off
  4. customdried under reduced pressure
  5. customThe residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2)

出典と根拠

ORDレコード
ord-1653111f11c149c6a8b3a71879c27fb2
出典データセット
uspto-grants-2013_11
特許番号
US08580778B2

反応ノート

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