5-Nitroso-2,4,6-pyrimidinetriamine → 2,4,7-Triamino-6-(2-chlorophenyl)pteridine

HRID 440890

반응식

HRID 440890 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([N:9]=O)=[C:4]([NH2:11])[N:3]=1.[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[CH2:19][C:20]#[N:21].C[O-].[Na+]>CN(C)C=O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]2[C:4](=[N:11][C:20]([NH2:21])=[C:19]([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[Cl:12])[N:9]=2)[N:3]=1

참가 물질

5

반응물 3

HCID 705045-Nitroso-2,4,6-pyrimidinetriamineHCID 76112(o-Chlorophenyl)acetonitrileHCID 10942334Sodium Methoxide

생성물 1

HCID 152789352,4,7-Triamino-6-(2-chlorophenyl)pteridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred solution of 1.5 grams (0.010 mole) of 2,4,6-triamino-5-nitrosopyrimidine in 80 mL of N,N-dimethylformamide was heated to reflux, and 2.0 grams (0.01 3 mole) of 2-chlorophenylacetonitrile was added in one portion. Upon completion of addition, the reaction mixture was cooled, and 0.7 gram (0.013 mole) of sodium methoxide was added in one portion. The reaction mixture was again heated at reflux for 15 minutes. The reaction mixture was cooled in an ice-bath and then was filtered to collect a solid. The solid was slurried in diethyl ether and then was again collected by filtration, yielding, when dried, 2.5 grams of 2,4,7-triamino-6-(2-chlorophenyl)pteridine. The NMR spectrum was consistent with the proposed structure.

후처리

  1. temperatureto reflux
  2. additionUpon completion of addition
  3. temperaturethe reaction mixture was cooled
  4. temperatureThe reaction mixture was again heated
  5. temperatureat reflux for 15 minutes
  6. temperatureThe reaction mixture was cooled in an ice-bath
  7. filtrationwas filtered
  8. customto collect a solid
  9. filtrationwas again collected by filtration
  10. customyielding
  11. customwhen dried

출처 및 근거

ORD 기록
ord-026491380cda4feb8509110ad50d91ee
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521190

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