Hydrochloric Acid → HCID 21948386、化合物

HRID 1276289ノート

反応式

HRID 1276289 の反応式
Cl.[NH2:2][C:3]1[N:8]=[C:7]([CH3:9])[C:6]([C:10]2[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.Cl.[CH3:20]O>>[NH2:2][C:3]1[N:8]=[C:7]([CH3:9])[C:6]([C:10]2[CH:18]=[CH:17][C:13]([C:14]([O:16][CH3:20])=[O:15])=[CH:12][CH:11]=2)=[CH:5][CH:4]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 70295713HCID 70295713、化合物

生成物 1

HCID 21948386HCID 21948386、化合物収率 70%

実験手順

A stirred suspension of 4-(6-amino-2-methylpyridin-3-yl)benzoic acid hydrochloride (D6, 1.9 g, 8.3 mmole) in methanol (120 ml) was treated with conc. HCl acid (1 ml) and heated under reflux for 2 h. The solution was concentrated in vacuo, the residue treated with excess 10% Na2CO3 solution and extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated in vacuo to afford the title compound as a pale yellow solid (1.4 g, 70%).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 2 h
  3. concentrationThe solution was concentrated in vacuo
  4. additionthe residue treated with excess 10% Na2CO3 solution
  5. extractionextracted with ethyl acetate
  6. dry with materialThe extract was dried (Na2SO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-449625e405d44150b6051e2c4e4a8e2f
出典データセット
uspto-grants-2000_12
特許番号
US06166034

反応ノート

読み込み中…