Sodium Hydroxide → 2-(1-Piperazinyl)-4-amino-6,7-dimethoxyquinazoline

HRID 1414237노트

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HRID 1414237 반응식
Br.[NH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[NH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=2)[N:12]=[C:11](Cl)[N:10]=1.[OH-].[Na+]>COCCO.O>[NH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=2)[N:12]=[C:11]([N:2]2[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]2)[N:10]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 3014804Piperazine--hydrogen bromide (1/1)

생성물 1

HCID 6162672-(1-Piperazinyl)-4-amino-6,7-dimethoxyquinazoline

시약·촉매·용매 2

HCID 962Water용매HCID 80192-Methoxyethanol용매

반응 조건

온도
75 °C

실험 절차

Piperazine hydrobromide (168.0 g., 1.006 mole) was added to a suspension of 4-amino-2-chloro-6,7-dimethoxyquinazoline (241.0 g., 1.006 mole) in 2-methoxyethanol (3.6 l.) and the mixture was stirred at reflux for 1.25 hours. The precipitate was separated by filtration, washed with hot 2-methoxyethanol and dried. The material then was added to a stirred solution of sodium hydroxide (81.0 g., 2.01 mole) in water (3 l.) and the mixture was heated to 75° C. The mixture then was cooled to 40° C., filtered, and the insoluble precipitate washed with water and dried. The material was triturated under refluxing absolute ethanol (6.0 l.) and the mixture was filtered. The filtrate was evaporated to dryness to yield the title compound, 180.0 g. (62%), M.P. 224°-228° C.

후처리

  1. temperatureat reflux for 1.25 hours
  2. customThe precipitate was separated by filtration
  3. washwashed with hot 2-methoxyethanol
  4. customdried
  5. temperatureThe mixture then was cooled to 40° C.
  6. filtrationfiltered
  7. washthe insoluble precipitate washed with water
  8. customdried
  9. customThe material was triturated
  10. temperatureunder refluxing absolute ethanol (6.0 l.)
  11. filtrationthe mixture was filtered
  12. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-c8156cdc59b7426ba17db8c58dbc4bca
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001238

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