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Methanol → 2,4-Dimethyl-3-[[2-methyl-5-(4-oxo-1-piperidyl)benzoyl]amino]benzoic acid

HRID 1427108
ノート
印刷プレビュー

反応式

HRID 1427108 の反応式
[OH-].[Na+].[CH3:3][C:4]1[C:13]([NH:14][C:15](=[O:30])[C:16]2[CH:21]=[C:20]([N:22]3[CH2:27][CH2:26][C:25](=[O:28])[CH2:24][CH2:23]3)[CH:19]=[CH:18][C:17]=2[CH3:29])=[C:12]([CH3:31])[CH:11]=[CH:10][C:5]=1[C:6]([O:8]C)=[O:7].CO>C1COCC1>[CH3:3][C:4]1[C:13]([NH:14][C:15](=[O:30])[C:16]2[CH:21]=[C:20]([N:22]3[CH2:27][CH2:26][C:25](=[O:28])[CH2:24][CH2:23]3)[CH:19]=[CH:18][C:17]=2[CH3:29])=[C:12]([CH3:31])[CH:11]=[CH:10][C:5]=1[C:6]([OH:8])=[O:7]
参加物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 887MethanolHCID 14798Sodium HydroxideHCID 86707338Methyl 2,4-dimethyl-3-[[2-methyl-5-(4-oxo-1-piperidyl)benzoyl]amino]benzoate

生成物 1

HCID 867073402,4-Dimethyl-3-[[2-methyl-5-(4-oxo-1-piperidyl)benzoyl]amino]benzoic acid収率 50.12%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of aqueous 2N NaOH (1.00 ml) is added to a stirred solution of methyl 2,4-dimethyl-3-[[2-methyl-5-(4-oxo-1-piperidyl)benzoyl]amino]benzoate (0.12 g, 304.20 μmol) in THF:MeOH (2 ml:1 ml). After 16 hours at ambient temperature, the organic solvent is removed under reduced pressure and the residue is diluted with water, acidified to pH 6 with 1N HCl, and extracted with ethyl acetate. The organic layers are combined with aqueous layer and concentrated under reduced pressure. The resulting solids are dissolved in acetonitrile/H2O and lyophilized to afford the title compound as an off-white solid (58 mg, 50.12%). Mass spectrum (m/z): 381.2 (M+1).

後処理

  1. customthe organic solvent is removed under reduced pressure
  2. additionthe residue is diluted with water
  3. extractionextracted with ethyl acetate
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe resulting solids are dissolved in acetonitrile/H2O

出典と根拠

ORDレコード
ord-ae081c9bf3c648aaab93b03426b579eb
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933098B2

反応ノート

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