Sodium Hydroxide → 2-(2-chloro-6-methoxy-phenyl)-3H-quinazolin-4-one

HRID 2079306

反応式

HRID 2079306 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11](=O)[C:12]1[C:17]([O:18][CH3:19])=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:20])(=[O:3])[NH2:2].[OH-].[Na+]>C(O)(=O)C>[Cl:20][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([O:18][CH3:19])[C:12]=1[C:11]1[NH:2][C:1](=[O:3])[C:4]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:10]=1

参加物

4

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 58010809N-(2-carbamoylphenyl)-2-chloro-6-methoxybenzamide

生成物 1

HCID 1361216082-(2-chloro-6-methoxy-phenyl)-3H-quinazolin-4-one収率 14%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

N-(2-carbamoylphenyl)-2-chloro-6-methoxybenzamide (13 g, 42.7 mmol) was suspended in 100 mL of a 2 N NaOH solution and heated to reflux. After refluxing for 3 hours, another 25 mL of a 2 N NaOH solution was added, and the reaction was refluxed for another hour. The mixture was cooled to room temperature and acidified with acetic acid to pH 5. The formed precipitate was collected by filtration. The product was purified over alumina using EtOAc as an eluent giving 1.7 g (5.9 mmol, 14%) of 2-(2-chloro-6-methoxy-phenyl)-3H-quinazolin-4-one.

後処理

  1. temperatureheated to reflux
  2. temperatureAfter refluxing for 3 hours
  3. temperaturethe reaction was refluxed for another hour
  4. filtrationThe formed precipitate was collected by filtration
  5. customThe product was purified over alumina

出典と根拠

ORDレコード
ord-63d7c787c42241aaa8a812e5bd29591e
出典データセット
uspto-grants-2011_04
特許番号
US07928107B2

関連ノート

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