Ethyl cyanoacetate → 3-Amino-1-(4-bromobenzyl)-pyrazol-5one

HRID 460884

反応式

HRID 460884 の反応式
[Na].C([O:4][C:5](=O)[CH2:6][C:7]#[N:8])C.[Br:10][C:11]1[CH:19]=[CH:18][C:14]([CH2:15][NH:16][NH2:17])=[CH:13][CH:12]=1>C(O)C>[NH2:8][C:7]1[NH:17][N:16]([CH2:15][C:14]2[CH:18]=[CH:19][C:11]([Br:10])=[CH:12][CH:13]=2)[C:5](=[O:4])[CH:6]=1

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 5360545SodiumHCID 167731114-Bromobenzylhydrazine

生成物 1

HCID 203672113-Amino-1-(4-bromobenzyl)-pyrazol-5one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
60 °C

実験手順

9.2 g of metallic sodium are dissolved in 200 ml of ethanol. A mixture of 25 g of cyanoacetic acid ethyl ester and 35 g of p-bromobenzylhydrazine in 50 ml of ethanol is then added at room temperature. The mixture is warmed to 60° C for 2 hours, the substance which was precipitated is filtered off and the filtrate is evaporated. The residue is taken up with water, the mixture is shaken with ether and the aqueous phase is acidified with dilute acetic acid. The crude product is purified by twice recrystallising it from alcohol.

後処理

  1. additionis then added at room temperature
  2. customthe substance which was precipitated
  3. filtrationis filtered off
  4. customthe filtrate is evaporated
  5. customThe crude product is purified
  6. customby twice recrystallising it from alcohol

出典と根拠

ORDレコード
ord-ce92e638c0bd4fd6a58ec88837c26c12
出典データセット
uspto-grants-1977_12
特許番号
US04061653

関連ノート

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