Hydrochloric Acid → 2-(3-Chlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylic acid

HRID 422040

反応式

HRID 422040 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:21]=[CH:22][CH:23]=1)[CH2:5][C:6]1[NH:15][C:14](=[O:16])[C:13]2[C:8](=[CH:9][C:10]([C:17]([O:19]C)=[O:18])=[CH:11][CH:12]=2)[N:7]=1.[OH-].[Na+].C(O)C.Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:21]=[CH:22][CH:23]=1)[CH2:5][C:6]1[NH:15][C:14](=[O:16])[C:13]2[C:8](=[CH:9][C:10]([C:17]([OH:19])=[O:18])=[CH:11][CH:12]=2)[N:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 136330125Methyl 2-(3-chlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate

生成物 1

HCID 1358172382-(3-Chlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylic acid収率 93.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 336 mg of methyl 2-(3-chlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate which was synthesized in Production Example 1, 3.0 mL of aqueous 1N sodium hydroxide solution and 6 mL of ethanol was heated for 2.5 hours under reflux. The reaction solution was allowed to cool off, and to which 3.0 mL of 1N hydrochloric acid and 5 mL of water were added. Whereupon precipitated crystals were recovered by filtration, washed with water and through-flow dried under heating, to provide 300 mg of the title compound.

後処理

  1. temperaturewas heated for 2.5 hours
  2. temperatureunder reflux
  3. temperatureto cool off
  4. customWhereupon precipitated crystals
  5. filtrationwere recovered by filtration
  6. washwashed with water
  7. customthrough-flow dried
  8. temperatureunder heating

出典と根拠

ORDレコード
ord-3d5e8ce669e14a9e8fee0c9c62f70618
出典データセット
uspto-grants-2012_01
特許番号
US08101624B2

関連ノート

読み込み中…