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

HRID 460884

반응식

HRID 460884 반응식
[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

참가 물질

5

반응물 3

HCID 7764Ethyl cyanoacetateHCID 5360545SodiumHCID 167731114-Bromobenzylhydrazine

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ce92e638c0bd4fd6a58ec88837c26c12
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061653

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