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Potassium Carbonate → N-(3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-4-(2-(tetrahydrofuran-2-yl)ethyl)-7,8-dihydro-5H-pyrano[4,3-d]pyrimidin-2-amine

HRID 1930700
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HRID 1930700 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:15][C:16]([NH2:18])=[NH:17])[CH:6]=[CH:7][C:8]=1[N:9]1[CH:13]=[C:12]([CH3:14])[N:11]=[CH:10]1.C(=O)([O-])[O-].[K+].[K+].[O:25]1[CH2:29][CH2:28][CH2:27][CH:26]1[CH2:30][CH2:31][C:32]([CH:34]1[C:39](=O)[CH2:38][CH2:37][O:36][CH2:35]1)=O>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:15][C:16]2[N:18]=[C:32]([CH2:31][CH2:30][CH:26]3[CH2:27][CH2:28][CH2:29][O:25]3)[C:34]3[CH2:35][O:36][CH2:37][CH2:38][C:39]=3[N:17]=2)[CH:6]=[CH:7][C:8]=1[N:9]1[CH:13]=[C:12]([CH3:14])[N:11]=[CH:10]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 593337093-(3-(tetrahydrofuran-2-yl)propanoyl)dihydro-2H-pyran-4(3H)-oneHCID 178493227HCID 178493227, 화합물

생성물 1

HCID 59333806N-(3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-4-(2-(tetrahydrofuran-2-yl)ethyl)-7,8-dihydro-5H-pyrano[4,3-d]pyrimidin-2-amine수율 1.1%

시약·촉매·용매 1

HCID 702
Ethanol
용매

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온도
50 °C

실험 절차

A reaction mixture of 1-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)guanidine (0.305 g, 0.83 mmol, example 7c) and potassium carbonate (0.343 g, 2.48 mmol) in ethanol (3 mL) was stirred at 50° C. for 20 minutes under argon. 3-(3-(tetrahydrofuran-2-yl)propanoyl)dihydro-2H-pyran-4(3H)-one (0.187 g, 0.83 mmol) was added dropwise (neat) over 2 hours and stirred at 50° C. overnight. The solvent was evporated and the residue was partitioned between water and dichloromethane. The water phase was extracted twice with dichloromethane. The combined organic layer was dried over MgSO4, filtered and concentrated. ¼ of the crude was purified by preparative HPLC and concentrated. The residue was partitioned between NaHCO3 (aq) and dichloromethane and the the water phase was extracted twice with dichloromethane, dried (MgSO4) and concentrated giving 4 mg of the product.

후처리

  1. stirringstirred at 50° C. overnight
  2. customthe residue was partitioned between water and dichloromethane
  3. extractionThe water phase was extracted twice with dichloromethane
  4. dry with materialThe combined organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customwas purified by preparative HPLC
  8. concentrationconcentrated
  9. customThe residue was partitioned between NaHCO3 (aq) and dichloromethane
  10. extractionthe the water phase was extracted twice with dichloromethane
  11. dry with materialdried (MgSO4)
  12. concentrationconcentrated

출처 및 근거

ORD 기록
ord-27d7c325335b4ac9822641de35232ed9
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188101B2

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