Sodium Hydroxide → 6-(Benzyloxy)-4-chloro-7-methoxyquinazoline

HRID 1008339노트

반응식

HRID 1008339 반응식
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([O:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][C:23]=1[O:24][CH3:25])[N:20]=[CH:19][NH:18][C:17]2=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(C(C)C)CC)(C)C.[OH-].[Na+]>>[CH2:6]([O:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][C:23]=1[O:24][CH3:25])[N:20]=[CH:19][N:18]=[C:17]2[Cl:3])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 4

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 1354970176-(Benzyloxy)-7-methoxyquinazolin-4(1H)-one

생성물 1

HCID 114265806-(Benzyloxy)-4-chloro-7-methoxyquinazoline수율 72%

실험 절차

Phosphorus oxychloride (3.1 ml) was added to 6-(benzyloxy)-7-methoxy-3,4-dihydro-4-quinazolinone (3.5 g) and diisopropylethylamine (11.5 ml). The mixture was refluxed for 20 min. The reaction solution was cooled to room temperature, and a 10% aqueous sodium hydroxide solution was then added to the cooled reaction solution, followed by extraction with chloroform. The organic layer was dried over sodium sulfate. The organic layer was filtered, and the solvent was then removed by distillation under the reduced pressure. The residue was dried through a vacuum pump to give 2.9 g (yield 72%) of the title compound.

후처리

  1. temperatureThe mixture was refluxed for 20 min
  2. extractionfollowed by extraction with chloroform
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationThe organic layer was filtered
  5. customthe solvent was then removed by distillation under the reduced pressure
  6. customThe residue was dried through a vacuum pump

출처 및 근거

ORD 기록
ord-82ee696a400b4a85a000176fe8e50fb1
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06797823B1

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