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1,4-Dioxane → HCID 54028232, 화합물

HRID 354010
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HRID 354010 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([O:31][CH3:32])[CH:30]=1)[CH2:6][N:7]([CH3:27])[C:8]([C:10]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[CH:14][N:13]=[C:12](S(C)(=O)=O)[N:11]=1)=[O:9].O1[CH2:38][CH2:37]OCC1>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([O:31][CH3:32])[CH:30]=1)[CH2:6][N:7]([CH3:27])[C:8]([C:10]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[CH:14][N:13]=[C:12]([N:11]2[CH2:38][CH2:37][N:7]([CH3:6])[CH2:8][CH2:10]2)[N:11]=1)=[O:9]
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반응물 2

HCID 312751,4-DioxaneHCID 536751832-Methanesulfonyl-5-o-tolyl-pyrimidine-4-carboxylic acid (3,5-dimethoxy-benzyl)-methyl-amide

생성물 1

HCID 54028232HCID 54028232, 화합물수율 168.2%

실험 절차

To a solution of 0.18 g (0.4 mmol) 2-methanesulfonyl-5-o-tolyl-pyrimidine-4-carboxylic acid (3,5-dimethoxy-benzyl)-methyl-amide in 10 ml dioxane 0.11 ml (0.99 mmol) 1-methylpiperazine was added. The reaction mixture was stirred for 16 hrs. After evaporation of the solvent, the residue was distributed between 50 ml CH2Cl2 and 50 ml H2O. The aqueous layer was extracted with 50 ml CH2Cl2, the combined organic layers dried (MgSO4), filtered and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2/MeOH/NH4OH 110:10:1) to give 0.16 g (85%) 2-(4-methyl-piperazin-1-yl)-5-o-tolyl-pyrimidine-4-carboxylic acid (3,5-dimethoxy-benzyl)-methyl-amide as a colorless foam, MS (ISP): 476.3 (M+H+).

후처리

  1. customAfter evaporation of the solvent
  2. extractionThe aqueous layer was extracted with 50 ml CH2Cl2
  3. dry with materialthe combined organic layers dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by chromatography (SiO2, CH2Cl2/MeOH/NH4OH 110:10:1)

출처 및 근거

ORD 기록
ord-240a74fddfe24e8a930a4c662450b501
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06756380B1

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