Nitric Acid → 6-Chloro-1,3-dimethyl-5-nitropyrimidine-2,4(1h,3h)-dione

HRID 648886노트

반응식

HRID 648886 반응식
S(=O)(=O)(O)O.[Cl:6][C:7]1[N:12]([CH3:13])[C:11](=[O:14])[N:10]([CH3:15])[C:9](=[O:16])[CH:8]=1.[N+:17]([O-])([OH:19])=[O:18]>>[Cl:6][C:7]1[N:12]([CH3:13])[C:11](=[O:14])[N:10]([CH3:15])[C:9](=[O:16])[C:8]=1[N+:17]([O-:19])=[O:18]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 814426-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 2496456-Chloro-1,3-dimethyl-5-nitropyrimidine-2,4(1h,3h)-dione수율 70%

실험 절차

To 25 ml of sulfuric acid was slowly added 8.5 g (0.049 mol) of 6-chloro-1,3-dimethyluracil as prepared in Synthesis Example 1 at 10° to 15° C. To this solution was gradually added 8.5 ml of fuming nitric acid at 0° to 5° C. After stirring for 5 minutes, the reaction mixture was poured onto ice and extracted twice with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The resulting crystals were recrystallized from a mixed solvent of ethyl acetate and hexane to give 7.5 g (70%) of 6-chloro-1,3-dimethyl-5-nitrouracil having a melting point of 91° to 92° C.

후처리

  1. customas prepared in Synthesis Example 1 at 10° to 15° C
  2. customat 0° to 5° C
  3. additionthe reaction mixture was poured onto ice
  4. extractionextracted twice with chloroform
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe resulting crystals were recrystallized from a mixed solvent of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-a25819ccd7b148d29581118983822033
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737442

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