Potassium Carbonate → 2,4-Diamino-6-(3,4-dichlorophenyl)-7-methylpteridine

HRID 440889

反応式

HRID 440889 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([N:9]=O)=[C:4]([NH2:11])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:18][C:19]1[CH:20]=[C:21]([CH2:26][C:27](=O)[CH3:28])[CH:22]=[CH:23][C:24]=1[Cl:25]>CN(C)C=O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]2[C:4](=[N:11][C:27]([CH3:28])=[C:26]([C:21]3[CH:22]=[CH:23][C:24]([Cl:25])=[C:19]([Cl:18])[CH:20]=3)[N:9]=2)[N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 705045-Nitroso-2,4,6-pyrimidinetriamineHCID 810603',4'-Dichloropropiophenone

生成物 1

HCID 152789342,4-Diamino-6-(3,4-dichlorophenyl)-7-methylpteridine収率 22.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A stirred solution of 1.0 gram (0.007 mole) of 2,4,6-triamino-5-nitrosopyrimidine and 2.7 grams (0.020 mole) of potassium carbonate in 30 mL of N,N-dimethylformamide was heated to 95°-100° C., and 2.0 grams (0.010 mole) of (3,4-dichlorophenyl)acetone was added in one portion. Upon completion of addition, the reaction mixture was allowed to cool to ambient temperature, where it was allowed to stir for about 18 hours. After this time the reaction mixture was concentrated under reduced pressure. The residue was triturated with 250 mL of water, and the remaining solid was collected by filtration. The solid was further triturated with 50 mL of 20% methanol in methylene chloride. The remaining solid was collected by filtration, yielding 0.5 gram of 2,4-diamino-6-(3,4-dichlorophenyl)-7-methylpteridine. The NMR spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of addition
  2. concentrationAfter this time the reaction mixture was concentrated under reduced pressure
  3. customThe residue was triturated with 250 mL of water
  4. filtrationthe remaining solid was collected by filtration
  5. customThe solid was further triturated with 50 mL of 20% methanol in methylene chloride
  6. filtrationThe remaining solid was collected by filtration

出典と根拠

ORDレコード
ord-b901b2e7e8994ba99bd679ddf6ed22aa
出典データセット
uspto-grants-1996_05
特許番号
US05521190

関連ノート

読み込み中…