Ethyl 2-methylacetoacetate → HCID 178433908、化合物

HRID 514326

反応式

HRID 514326 の反応式
[NH:1]([C:3]1[CH:8]=[C:7]([C:9]#[N:10])[CH:6]=[CH:5][N:4]=1)[NH2:2].C([O:13][C:14](=O)[CH:15]([CH3:19])[C:16](=O)[CH3:17])C>CCO.CC(O)=O>[OH:13][C:14]1[N:1]([C:3]2[CH:8]=[C:7]([C:9]#[N:10])[CH:6]=[CH:5][N:4]=2)[N:2]=[C:16]([CH3:17])[C:15]=1[CH3:19]

参加物

5

反応物 2

HCID 701Ethyl 2-methylacetoacetateHCID 201187142-Hydrazinylpyridine-4-carbonitrile

生成物 1

HCID 178433908HCID 178433908、化合物収率 47%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2-hydrazinylpyridine-4-carbonitrile (134 mg, 1 mmol, PREPARATION 2) and 2-methyl-3-oxo-butyric acid ethyl ester (158 mg, 1.1 mmol) in EtOH (5 mL) and AcOH (1 mL) was stirred at 90° C. overnight. The reaction mixture was cooled, concentrated, and purified by flash column chromatography (CH2Cl2) to afford the title compound (100 mg, 47%) as an orange solid. [M+H] Calc'd for C11H10N4O, 215. Found, 215.

後処理

  1. temperatureThe reaction mixture was cooled
  2. concentrationconcentrated
  3. custompurified by flash column chromatography (CH2Cl2)

出典と根拠

ORDレコード
ord-1bc84d3b06184c8582c335a76ca23ee2
出典データセット
uspto-grants-2015_08
特許番号
US09107916B2

関連ノート

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