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

HRID 1791995노트

반응식

HRID 1791995 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-af7ad205287341fbbed303d22e378a13
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07074798B2

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