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Undec-4-ene → HCID 54373433, 화합물

HRID 1756789
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HRID 1756789 반응식
[NH2:1][C:2]1[C:3]([N:10]([CH3:12])[CH3:11])=[N:4][CH:5]=[N:6][C:7]=1[O:8][CH3:9].C([O:15][C:16]([NH:18][CH2:19][C@@H:20]([C:26]1[CH:31]=[CH:30][CH:29]=[C:28]2[O:32][CH2:33][O:34][C:27]=12)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=O)C.[CH3:35]CCCCCC=CCCC>O1CCOCC1>[CH2:33]1[O:32][C:28]2[C:27](=[C:26]([C@@H:20]([CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:19][NH:18][C:16]([NH:1][C:2]3[C:3]([N:10]([CH3:11])[CH3:12])=[N:4][CH:5]=[N:6][C:7]=3[O:8][CH2:9][CH3:35])=[O:15])[CH:31]=[CH:30][CH:29]=2)[O:34]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 136496Undec-4-eneHCID 104195636-methoxy-4-N,4-N-dimethylpyrimidine-4,5-diamineHCID 54392650HCID 54392650, 화합물

생성물 1

HCID 54373433HCID 54373433, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A mixture of 0.66 g of 5-amino-4-dimethylamino-6-methoxypyrimidine, 1.28 g of N-ethoxycarbonyl-(R)-2-(2, 3-methylenedioxyphenyl) heptylamine, 0.55 g of 1, 8-diazabicyclo [5, 4, 0] undec-7-ene and 10 ml of dioxane was stirred at 100° C. for 16 hours and the solvent evaporated. The residue was chromatographed on a silica gel column, eluting with ethyl acetate-n-hexane (2:1-3:1), and the product was dissolved in ether. The solution was washed with water and saturated saline in this order, dried over anhydrous sodium sulfate and the solvent evaporated. The residue was triturated with n-hexane to give 0.63 g of the titled compound.

후처리

  1. customthe solvent evaporated
  2. customThe residue was chromatographed on a silica gel column
  3. washeluting with ethyl acetate-n-hexane (2:1-3:1)
  4. dissolutionthe product was dissolved in ether
  5. washThe solution was washed with water and saturated saline in this order
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent evaporated
  8. customThe residue was triturated with n-hexane

출처 및 근거

ORD 기록
ord-e41dc2650e004e7ca4d7022b86c1fc4b
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05442060

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