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

HRID 440889

반응식

HRID 440889 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b901b2e7e8994ba99bd679ddf6ed22aa
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521190

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