Water → 2,4,7-Triamino-6-(p-acetoxyphenyl)-pteridine

HRID 1414011노트

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HRID 1414011 반응식
[Na].[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([N:10]=O)=[C:5]([NH2:12])[N:4]=1.[C:13]([O:16][C:17]1[CH:25]=[CH:24][C:20]([CH2:21][C:22]#[N:23])=[CH:19][CH:18]=1)(=[O:15])[CH3:14].O>C(OCCO)C>[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]2[C:5](=[N:12][C:22]([NH2:23])=[C:21]([C:20]3[CH:19]=[CH:18][C:17]([O:16][C:13](=[O:15])[CH3:14])=[CH:25][CH:24]=3)[N:10]=2)[N:4]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 705045-Nitroso-2,4,6-pyrimidinetriamineHCID 5360545SodiumHCID 15628731p-Acetoxybenzylcyanide

생성물 1

HCID 205357152,4,7-Triamino-6-(p-acetoxyphenyl)-pteridine

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매2회

실험 절차

410 mg of metallic sodium are dissolved with stirring in 100 ml of 2-ethoxy-ethanol. 1100 mg of 2,4,6-triaminonitroso-pyrimidine and 1140 mg of p-acetoxybenzyl-cyanide are added with stirring one after the other and the mixture is heated to the boiling point with stirring. The color of the mixture changes from violet to brown. After two hours' boiling under reflux, heating is discontinued and the reaction mixture is left to cool. Subsequently, 70 to 80 percent of the 2-ethoxy-ethanol are drawn off using the vacuum from a water aspirator and the residue is combined with 500 ml of water. After extraction four times with ether, the extract is adjusted to pH 5 with 2 N hydrochloric acid. The precipitate is filtered off, washed with a little ice-cold acetone and recrystallized from 10 percent acetic acid. Further purification can follow using a silica gel column. The compound mentioned in the title is obtained, which compound decomposes (with charring) at 319°-321° C.

후처리

  1. temperatureis heated to the boiling point
  2. stirringwith stirring
  3. temperatureunder reflux
  4. temperatureheating
  5. waitthe reaction mixture is left
  6. temperatureto cool
  7. extractionAfter extraction four times with ether
  8. filtrationThe precipitate is filtered off
  9. washwashed with a little ice-cold acetone
  10. customrecrystallized from 10 percent acetic acid
  11. customFurther purification
  12. customis obtained
  13. customat 319°-321° C.

출처 및 근거

ORD 기록
ord-00a1921d900b400cb3818ded21b2320c
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04252809

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