6-Chloronicotinamide → HCID 12862365、化合物

HRID 904519ノート

反応式

HRID 904519 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([NH2:10])=[O:9])=[CH:4][CH:3]=1.[NH2:11][C:12]1[S:13][C:14]([CH:22]([CH3:24])[CH3:23])=[CH:15][C:16]=1[C:17](OCC)=[O:18]>CO>[CH3:24][CH:22]([C:14]1[S:13][C:12]2[N:11]=[C:2]3[CH:3]=[CH:4][C:5]([C:8]([NH2:10])=[O:9])=[CH:6][N:7]3[C:17](=[O:18])[C:16]=2[CH:15]=1)[CH3:23]

参加物

4

反応物 2

HCID 804566-ChloronicotinamideHCID 2756461ethyl 2-amino-5-isopropylthiophene-3-carboxylate

生成物 1

HCID 12862365HCID 12862365、化合物収率 20.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 24.0 g (0.1538 mol) of 6-chloro-3-pyridinecarboxamide (Aldrich Chemical Company) and 32.8 g (0.1538 mol) of 2-amino-5-(1-methylethyl)-3-thiophenecarboxylic acid, ethyl ester (Tetrahedron, Vol. 33, pages 2089-2092, 1977) is heated in a wax bath at 178°-182° C. for two hundred five minutes and then at 180°-196° C. for sixty-five minutes under nitrogen. The mixture is cooled, suspended in hot methanol and filtered to give 8.9 g of 2-(1-methylethyl)-4-oxo-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7-carboxamide; mp 280°-282° C. after recrystallization from dimethylformamide.

後処理

  1. temperatureis heated in a wax bath at 178°-182° C. for two hundred five minutes
  2. waitat 180°-196° C. for sixty-five minutes under nitrogen
  3. temperatureThe mixture is cooled
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-c60c8fa3a8924cc2b7a046ca378f7b6c
出典データセット
uspto-grants-1980_10
特許番号
US04230707

反応ノート

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