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Hydrochloric Acid → HCID 68196365、化合物

HRID 1626795
ノート
印刷プレビュー

反応式

HRID 1626795 の反応式
[OH:1][C:2]1[C:3]([C:34]([NH:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[O:35])=[N:4][C:5]([CH2:9][CH:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][C:23]4[CH:28]=[CH:27][C:26]([CH2:29][O:30][CH2:31][O:32]C)=[CH:25][CH:24]=4)=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)=[N:6][C:7]=1[CH3:8].Cl.O1CCOC[CH2:45]1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[C:31]([O:30][CH2:29][C:26]1[CH:27]=[CH:28][C:23]([CH2:22][C:19]2[CH:20]=[CH:21][C:16]([N:13]3[CH2:12][CH2:11][CH:10]([CH2:9][C:5]4[N:4]=[C:3]([C:34]([NH:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[O:35])[C:2]([OH:1])=[C:7]([CH3:8])[N:6]=4)[CH2:15][CH2:14]3)=[CH:17][CH:18]=2)=[CH:24][CH:25]=1)(=[O:32])[CH3:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 68196367HCID 68196367、化合物

生成物 1

HCID 68196365HCID 68196365、化合物収率 69%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl {[(5-hydroxy-2-{[1-(4-{4-[(methoxymethoxy)methyl]benzyl}phenyl)piperidin-4-yl]methyl}-6-methylpyrimidin-4-yl)carbonyl]amino}acetate (1.1 g, 1.9 mmol) was dissolved in ethyl acetate (14 mL), and a solution of hydrogen chloride in dioxane (4 M, 7 mL, 28 mmol) was added at room temperature, followed by stirring at the same temperature for 12 hours. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, followed by extraction with ethyl acetate, and subsequently the organic layer was dried over anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate), and a fraction corresponding to the Rf value=0.60 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (0.74 g, 1.3 mmol) as a yellow oil (yield 69%).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialsubsequently the organic layer was dried over anhydrous sodium sulfate
  3. distillationAfter the solvent was distilled off under reduced pressure
  4. customthe resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate)
  5. concentrationa fraction corresponding to the Rf value=0.60 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-2ef1e46930f14849a443631418b1ca26
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785462B2

反応ノート

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