Methyl Acrylate → Methyl 3-(2-amino-6-(2-furyl)-9H-purine-9-yl)propionate

HRID 271269

反応式

HRID 271269 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[NH:14][C:13]([NH2:15])=[N:12][C:11]2[C:7]=1[N:8]=[CH:9][N:10]=2.C([O-])([O-])=O.[K+].[K+].[C:22]([O:26][CH3:27])(=[O:25])[CH:23]=[CH2:24]>CN(C=O)C.CCOC(C)=O>[NH2:15][C:13]1[N:12]=[C:11]2[C:7]([N:8]=[CH:9][N:10]2[CH2:24][CH2:23][C:22]([O:26][CH3:27])=[O:25])=[C:6]([C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)[N:14]=1

参加物

6

反応物 3

HCID 7294Methyl AcrylateHCID 11430Potassium CarbonateHCID 1785082476-(furan-2-yl)-9H-purin-2-amine

生成物 1

HCID 59834959Methyl 3-(2-amino-6-(2-furyl)-9H-purine-9-yl)propionate収率 11.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 6-(2-furyl)-1H-purine-2-amine (0.70 g, 3.48 mmol) and K2CO3 (0.48 g, 3.48 mmol) in DMF (20 mL) was treated with methyl acrylate (3.3 g, 38.3 mmol), stirred for 40 h, diluted with EtOAc, filtered to remove polymeric acrylate, washed with water, dried (MgSO4), concentrated in vacuo and purified by chromatography [SiO2: EtOAc-heptane, (4:1)] to give the title compound (114 mg, 11%) as a white solid.

後処理

  1. filtrationfiltered
  2. customto remove polymeric acrylate
  3. washwashed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. custompurified by chromatography [SiO2: EtOAc-heptane, (4:1)]

出典と根拠

ORDレコード
ord-3c35fbd01a794b259e7c22e35a4be0c5
出典データセット
uspto-grants-2008_11
特許番号
US07452894B2

関連ノート

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