Ethanol → 4-(4-Amino-6,7-dimethoxyquinazolin-2-yl)piperazine-1-imidic Acid Ethyl Ester

HRID 461333노트

반응식

HRID 461333 반응식
[CH2:1]([OH:3])[CH3:2].[Na].[C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[N:22]=[C:21]([NH2:23])[C:20]3[C:15](=[CH:16][C:17]([O:26][CH3:27])=[C:18]([O:24][CH3:25])[CH:19]=3)[N:14]=2)[CH2:9][CH2:8]1)#[N:6]>C(O)(=O)C>[CH2:1]([O:3][C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[N:22]=[C:21]([NH2:23])[C:20]3[C:15](=[CH:16][C:17]([O:26][CH3:27])=[C:18]([O:24][CH3:25])[CH:19]=3)[N:14]=2)[CH2:9][CH2:8]1)=[NH:6])[CH3:2]

참가 물질

5

반응물 3

HCID 702EthanolHCID 5360545Sodium2회HCID 213933662-(4-Cyanopiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline

생성물 1

HCID 541908694-(4-Amino-6,7-dimethoxyquinazolin-2-yl)piperazine-1-imidic Acid Ethyl Ester

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a dry flask equipped with stirrer, thermometer and reflux condenser is placed 25 ml. of ethanol and sodium metal, 0.253 g. (0.011 g. atom) is added in portions. When the sodium is completely reacted, 3.14 g. (0.01 mole) of 2-(4-cyanopiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline is added and the resulting mixture is refluxed for 5 hours. After cooling to room temperature, glacial acetic acid is added to neutralize the mixture. After evaporation to dryness, 25 ml. of water and 50 ml. of chloroform are added to the residue. The mixture is transferred to a separatory funnel and the chloroform layer washed again with water, dried over anhydrous sodium sulfate then concentrated to dryness to provide the title compound.

후처리

  1. customTo a dry flask equipped with stirrer
  2. temperaturethermometer and reflux condenser
  3. addition(0.011 g. atom) is added in portions
  4. temperaturethe resulting mixture is refluxed for 5 hours
  5. customAfter evaporation to dryness, 25 ml
  6. additionof chloroform are added to the residue
  7. customThe mixture is transferred to a separatory funnel
  8. washthe chloroform layer washed again with water
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationthen concentrated to dryness

출처 및 근거

ORD 기록
ord-48208be7e38f41ac839ecf78dbd7004c
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062844

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