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Hydrazine hydrate (1:1) → 4-(6-Hydrazinylpyrimidin-4-yl)-1,4-oxazepane

HRID 562459
ノート
印刷プレビュー

反応式

HRID 562459 の反応式
O.[NH2:2][NH2:3].Cl[C:5]1[N:10]=[CH:9][N:8]=[C:7]([N:11]2[CH2:17][CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH:6]=1>C(O)C>[NH:2]([C:5]1[N:10]=[CH:9][N:8]=[C:7]([N:11]2[CH2:17][CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH:6]=1)[NH2:3]
参加物反応条件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 579250744-(6-Chloropyrimidin-4-yl)-1,4-oxazepane

生成物 1

HCID 579250704-(6-Hydrazinylpyrimidin-4-yl)-1,4-oxazepane

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, 8.8 ml (9.0 g, 180.2 mmol) of hydrazine hydrate are added dropwise with stirring to a solution of 3.9 g (18.0 mmol) of 4-(6-chloropyrimidin-4-yl)-1,4-oxazepane in 25 ml of ethanol. After 16 h of stirring at 80° C., the reaction solution is concentrated under reduced pressure. The residue is triturated with cold ethanol, the precipitated solid is filtered off and the filter residue is washed with 25 ml of diethyl ether. The product is dried under reduced pressure. Yield: 1.4 g (36% of theory)

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationthe reaction solution is concentrated under reduced pressure
  2. customThe residue is triturated with cold ethanol
  3. filtrationthe precipitated solid is filtered off
  4. washthe filter residue is washed with 25 ml of diethyl ether
  5. customThe product is dried under reduced pressure

出典と根拠

ORDレコード
ord-f3299233422f44ac851ba8cc88c80da6
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067407B2

反応ノート

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