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Chloroformamidinium chloride → 2,4-Diamino-5-methyl-6-[1-chloro-2-(4-trifluoromethylphenyl)ethenyl]quinazoline

HRID 363775
ノート
印刷プレビュー

反応式

HRID 363775 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=2)=[C:6]([CH3:22])[C:3]=1[C:4]#[N:5].[ClH:23].Cl[C:25]([NH2:27])=[NH:26]>COCCOCCOC.C(OCC)C>[NH2:27][C:25]1[N:26]=[C:4]([NH2:5])[C:3]2[C:2](=[CH:9][CH:8]=[C:7]([C:10]([Cl:23])=[CH:11][C:12]3[CH:17]=[CH:16][C:15]([C:18]([F:19])([F:20])[F:21])=[CH:14][CH:13]=3)[C:6]=2[CH3:22])[N:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3084509Chloroformamidinium chlorideHCID 541158512-Amino-6-methyl-5-[(4-trifluoromethylphenyl)ethynyl]benzonitrile

生成物 1

HCID 537897802,4-Diamino-5-methyl-6-[1-chloro-2-(4-trifluoromethylphenyl)ethenyl]quinazoline収率 46.9%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8150Diglyme溶媒

実験手順

This compound was prepared in a manner analogous to that of Step E of Example 1, using 2.7 grams (0.009 mole) of 2-amino-6-methyl-5-[(4-trifluoromethylphenyl)ethynyl]benzonitrile and 1.2 grams (0.011 mole) of chloroformamidine hydrochloride in 10 mL of 2-methoxyethyl ether. Upon completion of the reaction, the reaction mixture was diluted with 200 mL of diethyl ether. The resultant solid was collected by filtration, and was dissolved in a hot mixture of 300 mL of water and 100 mL of n-propanol. The solution was filtered hot through a sintered glass funnel to remove some insoluble material. The filtrate was then made basic with 100 mL of concentrated ammonium hydroxide. The resultant solid was collected by filtration, and dried at 60° C. under vacuum. The solid was then dissolved in a solution of 10% methanol in methylene chloride, and the solution was subjected to column chromatography on silica gel. Elution was accomplished using 10% methanol in methylene chloride. The product-containing fractions were combined and concentrated under reduced pressure, yielding 1.6 grams of 2,4-diamino-5-methyl-6-[1-chloro-2-(4-trifluoromethylphenyl)ethenyl]quinazoline, mp >300° C. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customThis compound was prepared in a manner analogous to that of Step E of Example 1
  2. customUpon completion of the reaction
  3. filtrationThe resultant solid was collected by filtration
  4. dissolutionwas dissolved in a hot mixture of 300 mL of water and 100 mL of n-propanol
  5. filtrationThe solution was filtered hot through a sintered glass funnel
  6. customto remove some insoluble material
  7. filtrationThe resultant solid was collected by filtration
  8. customdried at 60° C. under vacuum
  9. dissolutionThe solid was then dissolved in a solution of 10% methanol in methylene chloride
  10. washElution
  11. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f5a5a7a2eaa24d90be44ac378bc0424c
出典データセット
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05874579

反応ノート

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