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

HRID 1414237ノート

反応式

HRID 1414237 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80192-Methoxyethanol溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c8156cdc59b7426ba17db8c58dbc4bca
出典データセット
uspto-grants-1977_01
特許番号
US04001238

反応ノート

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