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

HRID 440890

反応式

HRID 440890 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.[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-026491380cda4feb8509110ad50d91ee
出典データセット
uspto-grants-1996_05
特許番号
US05521190

関連ノート

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