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4-[(1-Methyl-1H-pyrazol-3-yl)amino]quinazolin-6-ol → 6-{[3-chloro-5-(2-methoxyethoxy)pyridin-2-yl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)quinazoline-4-amine

HRID 81663
ノート
印刷プレビュー

反応式

HRID 81663 の反応式
Cl[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([O:9][CH2:10][CH2:11][O:12][CH3:13])=[CH:4][N:3]=1.CC(C)([O-])C.[K+].[CH3:20][N:21]1[CH:25]=[CH:24][C:23]([NH:26][C:27]2[C:36]3[C:31](=[CH:32][CH:33]=[C:34]([OH:37])[CH:35]=3)[N:30]=[CH:29][N:28]=2)=[N:22]1.O.[Cl-].[Na+]>C(Cl)(Cl)Cl.CN(C)C(=O)C>[Cl:8][C:7]1[C:2]([O:37][C:34]2[CH:35]=[C:36]3[C:31](=[CH:32][CH:33]=2)[N:30]=[CH:29][N:28]=[C:27]3[NH:26][C:23]2[CH:24]=[CH:25][N:21]([CH3:20])[N:22]=2)=[N:3][CH:4]=[C:5]([O:9][CH2:10][CH2:11][O:12][CH3:13])[CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 231603824-[(1-Methyl-1H-pyrazol-3-yl)amino]quinazolin-6-olHCID 23665647Potassium tert-butoxideHCID 57417360Sodium chloride; waterHCID 866459022,3-Dichloro-5-(2-methoxyethoxy)pyridine

生成物 1

HCID 595088886-{[3-chloro-5-(2-methoxyethoxy)pyridin-2-yl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)quinazoline-4-amine収率 28.1%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 31374Dimethylacetamide溶媒

反応条件

温度
180 °C

実験手順

2,3-Dichloro-5-(2-methoxyethoxy)pyridine (127 mg, 0.57 mmol) and potassium tert-butoxide (70 mg, 0.62 mmol) were added to an N,N-dimethylacetamide solution (2 ml) of 4-[(1-methyl-1H-pyrazol-3-yl)amino]quinazolin-6-ol (60 mg, 0.25 mmol), and stirred overnight at 180° C. under a nitrogen atmosphere in a sealed tube. The reaction solution was cooled with ice, then sodium chloride water and chloroform were added, the organic layer was washed with water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by reversed-phase liquid chromatography (YMC CombiPrep Pro C18 AS-360-CC) to obtain the entitled compound (30 mg, yield: 28%) as a pale orange amorphous solid.

後処理

  1. temperatureThe reaction solution was cooled with ice
  2. washthe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained residue was purified by reversed-phase liquid chromatography (YMC CombiPrep Pro C18 AS-360-CC)

出典と根拠

ORDレコード
ord-8cfc7015865c40fcbf15d36aa65d671e
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846700B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート