Ammonium Acetate → 5-methyl-2-oxo-1H-1,6-naphthyridine-3-carbonitrile

HRID 462711ノート

反応式

HRID 462711 の反応式
[C:1]([O-])(=O)C.[NH4+].C[N:7]([CH3:19])[CH:8]=[CH:9][C:10]1[NH:15][C:14](=[O:16])[C:13]([C:17]#[N:18])=[CH:12][CH:11]=1>CN(C)C=O>[CH3:1][C:19]1[N:7]=[CH:8][CH:9]=[C:10]2[C:11]=1[CH:12]=[C:13]([C:17]#[N:18])[C:14](=[O:16])[NH:15]2

参加物

4

反応物 2

HCID 517165Ammonium Acetate2 回HCID 541748101,2-Dihydro-6-(2-dimethylaminoethenyl)-2-oxo-3-pyridinecarbonitrile

生成物 1

HCID 57130685-methyl-2-oxo-1H-1,6-naphthyridine-3-carbonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
5 °C

実験手順

The above preparation was also carried out using ammonium acetate in place of formamidine acetate as follows: A mixture containing 1.305 kg of 1,2-dihydro-6-(2-dimethylaminoethenyl)-2-oxo-3-pyridinecarbonitrile, 9 liters of dimethylformamide and 915 g of ammonium acetate was refluxed for five hours The reaction suspension was cooled to 5° C. for three hours and the precipitated product was collected, washed twice with cold 60/40 by volume of dimethylformamide/water, twice with cold ethanol, once with ether and dried to yield 826 g of 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridine-3-carbonitrile, m.p. 75°-277° C.

後処理

  1. customThe above preparation
  2. temperaturewas refluxed for five hours The reaction suspension
  3. customthe precipitated product was collected
  4. washwashed twice with cold 60/40 by volume of dimethylformamide/water, twice with cold ethanol, once with ether
  5. customdried

出典と根拠

ORDレコード
ord-ab0a59d9a34c4c8fa883a7a325ff55bd
出典データセット
uspto-grants-1985_05
特許番号
US04517190

反応ノート

読み込み中…