Sodium Hydroxide → 2-chloro-7-methoxy-8-methyl-1H-quinazolin-4-one

HRID 1443490ノート

反応式

HRID 1443490 の反応式
[OH-:1].[Na+].[Cl:3][C:4]1[N:13]=[C:12](Cl)[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([O:15][CH3:16])=[CH:9][CH:10]=2)[N:5]=1>O.C1COCC1>[Cl:3][C:4]1[N:13]=[C:12]([OH:1])[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([O:15][CH3:16])=[CH:9][CH:10]=2)[N:5]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 591654322,4-Dichloro-7-methoxy-8-methylquinazoline

生成物 1

HCID 1784877522-chloro-7-methoxy-8-methyl-1H-quinazolin-4-one収率 99.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

A solution of NaOH (1.58 g, 39.6 mmol) in water (40 mL) was added to 2,4-dichloro-7-methoxy-8-methylquinazoline (139) (3.2 g, 13.05 mmol) in THF (20 mL). The resulting mixture was heated at 40° C. for 24 h. Then, the reaction mixture was cooled to room temperature, THF was evaporated and additional water (30 mL) was added. The precipitate was filtered off. Then, the pH of the filtrate was adjusted to 5 with AcOH to give a solid which was subsequently filtered off and successively washed with water and isopropylether to give the title compound (2.91 g, 99%) as a yellowish powder: m/z=225 (M+H)+.

後処理

  1. temperatureThen, the reaction mixture was cooled to room temperature
  2. customTHF was evaporated
  3. additionadditional water (30 mL) was added
  4. filtrationThe precipitate was filtered off
  5. customto give a solid which
  6. filtrationwas subsequently filtered off
  7. washsuccessively washed with water and isopropylether

出典と根拠

ORDレコード
ord-3ebf83711de04fe6829a5b30fbc2ae75
出典データセット
uspto-grants-2010_02
特許番号
US07659245B2

反応ノート

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