N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamide → N8-[4-(tert-butyl)-1,3-thiazol-2-yl]-2,4-dioxo-3,4-dihydro-2H-pyrido[1,2-a]pyrimidine-8-carboxamide

HRID 1828442ノート

反応式

HRID 1828442 の反応式
[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:19])[C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH2:18])[CH:13]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[C:20](OC1C=CC(Cl)=C(Cl)C=1Cl)(=[O:25])[CH2:21][C:22]([O-])=[O:23]>C1(C)C(C)=CC=CC=1>[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11]([C:12]2[CH:17]=[CH:16][N:15]3[C:20](=[O:25])[CH2:21][C:22](=[O:23])[N:18]=[C:14]3[CH:13]=2)=[O:19])[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 22063525N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamideHCID 22063717Trichlorophenyl malonate

生成物 1

HCID 22063754N8-[4-(tert-butyl)-1,3-thiazol-2-yl]-2,4-dioxo-3,4-dihydro-2H-pyrido[1,2-a]pyrimidine-8-carboxamide収率 84%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
130 °C

実験手順

N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamide (200 mg, 0.724 mmol) was added with xylene (20 ml) and trichlorophenyl malonate (370 mg, 0.796 mmol) and refluxed by heating at 130° C. The reaction solution was stirred for 1 hour, then returned to room temperature and concentrated under reduced pressure. The resulting orange crystals was taken by filtration, washed with chloroform, dried under reduced pressure to obtain 209 mg (84%) of the title compound as orange crystals without purification.

後処理

  1. temperaturerefluxed
  2. customreturned to room temperature
  3. concentrationconcentrated under reduced pressure
  4. filtrationThe resulting orange crystals was taken by filtration
  5. washwashed with chloroform
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-fcd8f059b5fe4effa3a35423e0f94982
出典データセット
uspto-grants-2006_06
特許番号
US07056917B2

反応ノート

読み込み中…