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Dimethylformamide → 8-methyl-5-methylsulfanyl-1,3-diphenyl-1H,8H-pyrimido[4,5-d]pyrimidine-2,4,7-trione

HRID 2224149
ノート
印刷プレビュー

反応式

HRID 2224149 の反応式
[SH:1][C:2]1[C:3]2[C:13](=[O:14])[N:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:11](=[O:21])[N:10]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:4]=2[N:5]([CH3:9])[C:6](=[O:8])[N:7]=1.[CH3:28]N(C)C=O.C(=O)([O-])[O-].[K+].[K+].CI>O>[CH3:9][N:5]1[C:4]2[N:10]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:11](=[O:21])[N:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:13](=[O:14])[C:3]=2[C:2]([S:1][CH3:28])=[N:7][C:6]1=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178481636HCID 178481636、化合物

生成物 1

HCID 597172888-methyl-5-methylsulfanyl-1,3-diphenyl-1H,8H-pyrimido[4,5-d]pyrimidine-2,4,7-trione収率 89%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

To crude 5-mercapto-8-methyl-1,3-diphenyl-1H,8H-pyrimido[4,5-d]pyrimidine-2,4,7-trione 24 (100 mg) obtained in Step 5 was added N,N-dimethylformamide (0.5 ml). Under a nitrogen atmosphere, potassium carbonate (44 mg) and methyl iodide 25 (20 μl) were successively added, and the mixture was stirred at room temperature for 3 hrs. Water was added, and the mixture was extracted with chloroform. The organic layer was washed with water and brine, and dried over anhydrous sodium sulfate. Anhydrous sodium sulfate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (hexane:ethyl acetate=4:1→3:1) to give 8-methyl-5-methylsulfanyl-1,3-diphenyl-1H,8H-pyrimido[4,5-d]pyrimidine-2,4,7-trione 26 (91 mg, yield 89%) as brown crystals.

後処理

  1. extractionthe mixture was extracted with chloroform
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate. Anhydrous sodium sulfate
  4. filtrationwas filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by column chromatography (hexane:ethyl acetate=4:1→3:1)

出典と根拠

ORDレコード
ord-e5bee5a4c46f4791844f62a676c7ad89
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07378423B2

反応ノート

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