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3-(3,4,5-Trimethoxyphenyl)acrylic acid → 3-Propyl-8-[2-(3,4,5-trimethoxy-phenyl)-vinyl]-3,7-dihydro-purine-2,6-dione

HRID 1292425
ノート
印刷プレビュー

反応式

HRID 1292425 の反応式
[NH2:1][C:2]1[C:3](=[O:13])[NH:4][C:5](=[O:12])[N:6]([CH2:9][CH2:10][CH3:11])[C:7]=1[NH2:8].C1(N=C=NC2CCCCC2)CCCCC1.ON1C2C=CC=CC=2N=N1.[CH3:39][O:40][C:41]1[CH:42]=[C:43]([CH:49]=[C:50]([O:54][CH3:55])[C:51]=1[O:52][CH3:53])[CH:44]=[CH:45][C:46](O)=O>CN(C)C=O>[CH2:9]([N:6]1[C:7]2[N:8]=[C:46](/[CH:45]=[CH:44]/[C:43]3[CH:49]=[C:50]([O:54][CH3:55])[C:51]([O:52][CH3:53])=[C:41]([O:40][CH3:39])[CH:42]=3)[NH:1][C:2]=2[C:3](=[O:13])[NH:4][C:5]1=[O:12])[CH2:10][CH3:11]
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 70213-(3,4,5-Trimethoxyphenyl)acrylic acidHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 106313415,6-Diamino-1-propyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

生成物 1

HCID 151708643-Propyl-8-[2-(3,4,5-trimethoxy-phenyl)-vinyl]-3,7-dihydro-purine-2,6-dione収率 60%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5,6-Diamino-1-propyluracil (2.00 g, 11 mmol) was suspended in 40 ml of N,N-dimethylformamide. To the suspension were added 3.37 g (16 mmol) of N,N'-dicyclohexylcarbodiimide and 2.00 g (13 mmol) of 1-hydroxybenzotriazole. Then, 2.59 g (11 mmol) of 3,4,5-trimethoxycinnamic acid was slowly added thereto in several portions, and the mixture was stirred overnight at room temperature. After insoluble substances were removed by filtration, the filtrate was concentrated under reduced pressure and 40 ml of a 2N aqueous solution of sodium hydroxide was added to the residue. The mixture was heated under reflux for 30 minutes, followed by neutralization. Deposited crystals were collected by filtration and recrystallized from isopropanol/water to give 2.51 g (overall yield: 60%) of Compound 22 as a yellow powder.

後処理

  1. customAfter insoluble substances were removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure and 40 ml of a 2N aqueous solution of sodium hydroxide
  3. additionwas added to the residue
  4. temperatureThe mixture was heated
  5. temperatureunder reflux for 30 minutes
  6. filtrationDeposited crystals were collected by filtration
  7. customrecrystallized from isopropanol/water

出典と根拠

ORDレコード
ord-038f24034db9491a8186406b565c0add
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05756735

反応ノート

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