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Citric Acid → Methyl 4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)-2-nitrobenzoate

HRID 454492
ノート
印刷プレビュー

反応式

HRID 454492 の反応式
[H-].[Na+].[C:3]([O:7][C:8]([NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23][CH3:24])=[O:22])=[C:19]([N+:27]([O-:29])=[O:28])[CH:18]=1)=[O:9])([CH3:6])([CH3:5])[CH3:4].CI.[C:32](O)(=O)CC(CC(O)=O)(C(O)=O)O>C(OCC)C.O.CN(C)C=O>[C:3]([O:7][C:8]([N:10]([CH3:32])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23][CH3:24])=[O:22])=[C:19]([N+:27]([O-:29])=[O:28])[CH:18]=1)=[O:9])([CH3:6])([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 311Citric AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 66989922Methyl 4-(2-(tert-butoxycarbonylamino)phenyl)-2-nitrobenzoate

生成物 1

HCID 66990621Methyl 4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)-2-nitrobenzoate

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 3283Diethyl Ether溶媒
HCID 6228Dimethylformamide溶媒

実験手順

Under ice-cooling, 60% sodium hydride (0.21 g) was added to an N,N-dimethylformamide (15 mL) solution of methyl 4-(2-(tert-butoxycarbonylamino)phenyl)-2-nitrobenzoate (1.3 g), followed by stirring at room temperature for 10 minutes. Then, methyl iodide (0.32 mL) was added thereto under ice-cooling, followed by stirring at room temperature for 1 hour. Water, a 10% aqueous solution of citric acid, and diethyl ether were added to the reaction mixture. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 95-85% hexane/ethyl acetate] to obtain 1.1 g of methyl 4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)-2-nitrobenzoate as a light yellow solid.

後処理

  1. temperatureUnder ice-cooling
  2. temperatureunder ice-cooling
  3. stirringby stirring at room temperature for 1 hour
  4. customThe organic layer was separated
  5. washwashed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography [eluent: 95-85% hexane/ethyl acetate]

出典と根拠

ORDレコード
ord-ace8e3bc5abb44e7807a4503e9326236
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

読み込み中…

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