Trifluoroacetic acid → 3-Methyl-8-piperazin-1-yl-7-prop-2-enylpurine-2,6-dione

HRID 1791995ノート

反応式

HRID 1791995 の反応式
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][N:18]([C:21]2[N:29]([CH2:30][CH:31]=[CH2:32])[C:28]3[C:27](=[O:33])[NH:26][C:25](=[O:34])[N:24]([CH3:35])[C:23]=3[N:22]=2)[CH2:17][CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[CH2:30]([N:29]1[C:28]2[C:27](=[O:33])[NH:26][C:25](=[O:34])[N:24]([CH3:35])[C:23]=2[N:22]=[C:21]1[N:18]1[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]1)[CH:31]=[CH2:32]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 235369544-(7-Allyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 6774233-Methyl-8-piperazin-1-yl-7-prop-2-enylpurine-2,6-dione収率 76.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (294 μl) was added dropwise to a solution of 4-(7-allyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester (150 mg) in methylene chloride (2 ml), and the reaction mixture was stirred at room temperature for 1 hour and 30 minutes. The solvent was removed by distillation at reduced pressure from the reaction mixture. The residue was subjected to azeotropic distillation with toluene, and then was purified by silica gel column chromatography to give 85 mg of the title compound from a fraction eluted with methanol-ethyl acetate (1:10).

後処理

  1. customThe solvent was removed by distillation at reduced pressure from the reaction mixture
  2. distillationThe residue was subjected to azeotropic distillation with toluene
  3. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-af7ad205287341fbbed303d22e378a13
出典データセット
uspto-grants-2006_07
特許番号
US07074798B2

反応ノート

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