1-Methyluracil → 5-(2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl)-1-methyl-2,4(3H)-pyrimidinedione

HRID 1872021노트

반응식

HRID 1872021 반응식
[CH3:1][C:2]1[CH:18]=[CH:17][C:5]2[CH:6](O)[C:7]3[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][C:8]=3[CH2:9][CH2:10][C:4]=2[CH:3]=1.[CH3:19][N:20]1[CH:27]=[CH:26][C:24](=[O:25])[NH:23][C:21]1=[O:22]>FC(F)(F)C(O)=O.O>[CH3:15][C:12]1[CH:13]=[CH:14][C:7]2[CH:6]([C:26]3[C:24](=[O:25])[NH:23][C:21](=[O:22])[N:20]([CH3:19])[CH:27]=3)[C:5]3[CH:17]=[CH:18][C:2]([CH3:1])=[CH:3][C:4]=3[CH:10]=[CH:9][C:8]=2[CH:11]=1

참가 물질

5

반응물 2

HCID 120091-MethyluracilHCID 1868974710,11-Dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-ol

생성물 1

HCID 186897095-(2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl)-1-methyl-2,4(3H)-pyrimidinedione

시약·촉매·용매 2

HCID 962Water용매HCID 6422Trifluoroacetic acid용매

실험 절차

To a solution of the product of step (i) (0.094 g) in trifluoroacetic acid (4 ml) under a nitrogen atmosphere was added 1-methyluracil (0.01 g), and the mixture stirred at room temperature for 1 hour. Evaporation of solvent afforded an orange oil which was azeotroped once with acetonitrile (5 ml). The crude product was redissolved in acetonitrile (2 ml), and stirred at room temperature for 0.5 h, giving a white precipitate. The reaction mixture was diluted with water (10 ml) and the white precipitate isolated by filtration. Yield: 0.085 g

후처리

  1. customEvaporation of solvent
  2. customafforded an orange oil which
  3. customwas azeotroped once with acetonitrile (5 ml)
  4. dissolutionThe crude product was redissolved in acetonitrile (2 ml)
  5. stirringstirred at room temperature for 0.5 h
  6. customgiving a white precipitate
  7. customthe white precipitate isolated by filtration

출처 및 근거

ORD 기록
ord-7b405762c5cb4a33ba410774fc7906ba
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107297

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