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Undec-4-ene → HCID 54373433、化合物

HRID 1756789
ノート
印刷プレビュー

反応式

HRID 1756789 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 136496Undec-4-eneHCID 104195636-methoxy-4-N,4-N-dimethylpyrimidine-4,5-diamineHCID 54392650HCID 54392650、化合物

生成物 1

HCID 54373433HCID 54373433、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e41dc2650e004e7ca4d7022b86c1fc4b
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05442060

反応ノート

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