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

HRID 271269

반응식

HRID 271269 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)]

출처 및 근거

ORD 기록
ord-3c35fbd01a794b259e7c22e35a4be0c5
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452894B2

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