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Acetic Acid → 4-(6-Methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde

HRID 604999
ノート
印刷プレビュー

反応式

HRID 604999 の反応式
[O:1]=[C:2]1[NH:11][CH:10]=[CH:9][C:8]2[N:7]=[C:6]([C:12]3[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=3)[C:5]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:4][C:3]1=2.[H-].[Na+].CI.[C:30](O)(=O)C>CN(C=O)C.C(OCC)(=O)C>[CH3:30][N:11]1[CH:10]=[CH:9][C:8]2[N:7]=[C:6]([C:12]3[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=3)[C:5]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:4][C:3]=2[C:2]1=[O:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 592646194-(5-Oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde

生成物 1

HCID 866249424-(6-Methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-(5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde (186 mg, 0.57 mmol) in dry DMF (2 mL) was added 60% sodium hydride in mineral oil (29 mg, 0.72 mmol). The reaction was stirred at room temperature for 15 minutes and then methyl iodide was added via syringe (40 μL, 0.70 mmol). After 30 minutes the reaction was diluted with ethyl acetate and some acetic acid was added to neutralize the base. The solution was washed with aqueous NaHCO3 and the organic layer was dried (anhydrous Na2SO4), filtered and the solvent evaporated. The residue was triturated with diethyl ether to give the title compound as a pale yellow solid. The mother liquors were chromatographed on silica gel eluting with a 30-70% ethyl acetate/hexane gradient to give additional product. 1H-NMR (500 MHz, CDCl3): δ 10.02 (1H, s), 8.74 (1H, s), 7.80 (2H, d, J=8 Hz), 7.60 (2H, d, J=8 Hz), 7.37 (1H, d, J=7.6 Hz), 7.28-7.31 (2H, m), 7.19-7.22 (2H, m), 6.85 (1H, d, J=7.6 Hz), 3.67 (3H, s). m/e (m+1): 341.1.

後処理

  1. washThe solution was washed with aqueous NaHCO3
  2. dry with materialthe organic layer was dried (anhydrous Na2SO4)
  3. filtrationfiltered
  4. customthe solvent evaporated
  5. customThe residue was triturated with diethyl ether

出典と根拠

ORDレコード
ord-789aed7ff6454838acf2c675b0cbb8a4
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07910561B2

反応ノート

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