Methanol → HCID 68869975、化合物

HRID 1985273ノート

反応式

HRID 1985273 の反応式
[C:1]([C:5]1[CH:35]=[CH:34][C:8]([CH2:9][N:10]2[CH2:14][CH:13]([CH2:15][CH2:16][CH2:17][C:18]3[CH:30]=[CH:29][C:21]([O:22][C:23]([CH3:28])([CH3:27])[C:24]([OH:26])=[O:25])=[C:20]([CH3:31])[CH:19]=3)[N:12]([CH3:32])[C:11]2=[O:33])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:36]O>S(=O)(=O)(O)O>[CH3:36][O:25][C:24](=[O:26])[C:23]([O:22][C:21]1[CH:29]=[CH:30][C:18]([CH2:17][CH2:16][CH2:15][CH:13]2[CH2:14][N:10]([CH2:9][C:8]3[CH:34]=[CH:35][C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])=[CH:6][CH:7]=3)[C:11](=[O:33])[N:12]2[CH3:32])=[CH:19][C:20]=1[CH3:31])([CH3:27])[CH3:28]

参加物

4

反応物 2

HCID 887MethanolHCID 10195632HCID 10195632、化合物

生成物 1

HCID 68869975HCID 68869975、化合物収率 99%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

To a solution of 2-(4-{3-[1-(4-tert-Butyl-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-propyl}-2-methyl-phenoxy)-2-methyl-propionic acid (0.610 g, 1.27 mmole) in methanol (10 mL) was added 15 drops of concentrated sulfuric acid. The mixture was stirred at room temperature overnight. After evaporated the solvent, the residue was partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was washed by saturated sodium bicarbonate (50 mL), then brine (3×50 mL), dried over Na2SO4, filtered and concentrated in vacuo to produce an oil (0.624 g, 99%). Mass [EI+] 495 (M+H)+.

後処理

  1. customAfter evaporated the solvent
  2. customthe residue was partitioned between ethyl acetate (50 mL) and water (50 mL)
  3. washThe organic layer was washed by saturated sodium bicarbonate (50 mL)
  4. dry with materialbrine (3×50 mL), dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2f91848927b448c1b084eb0b03b2558e
出典データセット
uspto-grants-2009_06
特許番号
US07544812B2

反応ノート

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