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Ethanol → Ethyl 6-[(4-chlorophenyl)methylcarbamoyl]-2-methoxy-8-methyl-5-oxo-1,8-naphthyridine-3-carboxylate

HRID 1280466
ノート
印刷プレビュー

反応式

HRID 1280466 の反応式
[Cl:1][C:2]1[CH:26]=[CH:25][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:19](=[O:20])[C:18]3[C:13](=[N:14][C:15]([O:22][CH3:23])=[C:16](I)[CH:17]=3)[N:12]([CH3:24])[CH:11]=2)=[O:9])=[CH:4][CH:3]=1.C1C=CC(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[CH2:56]([OH:58])[CH3:57].C(N(CC)CC)C.CN([CH:69]=[O:70])C>C(Cl)Cl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:26]=[CH:25][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:19](=[O:20])[C:18]3[CH:17]=[C:16]([C:69]([O:58][CH2:56][CH3:57])=[O:70])[C:15]([O:22][CH3:23])=[N:14][C:13]=3[N:12]([CH3:24])[CH:11]=2)=[O:9])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 702EthanolHCID 6228DimethylformamideHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 5276330N-[(4-chlorophenyl)methyl]-6-iodo-7-methoxy-1-methyl-4-oxo-1,8-naphthyridine-3-carboxamide

生成物 1

HCID 5276333
Ethyl 6-[(4-chlorophenyl)methylcarbamoyl]-2-methoxy-8-methyl-5-oxo-1,8-naphthyridine-3-carboxylate
収率 76%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

N-(4-Chlorobenzyl)-6-iodo-7-methoxy-1-methyl-4-oxo-1,4-dihydro[1,8]naphthyridine-3-carboxamide (700 mg), palladium acetate (32 mg), DPPP (60 mg), ethanol (10 mL) and triethylamine (1 mL) are dissolved in DMF (20 mL) in a steel bomb. The bomb is flushed with CO (3×) and then pressured with CO (400 psi) and the resulting reaction is stirred at 80° C. for 24 h, cooled to room temperature and diluted with CH2Cl2. The organic is washed with water, 1N HCl, brine, dried (MgSO4), filtered and concentrated in vacuo. The residue is purified by silica gel chromatography (CH2Cl2/MeOH 1/0, 45/1) and then triturated with MeOH to afford 472 mg (76%) of ethyl 6-{[(4-chlorobenzyl)amino]carbonyl}-2-methoxy-8-methyl-5-oxo-5,8-dihydro[1,8]naphthyridine-3-carboxylate. Physical characteristics are as follows: 1H NMR (CDCl3) δ 10.26-10.23, 9.18, 8.85, 7.32, 4.65, 4.40, 4.19, 4.00, 1.41; 13C NMR (CDCl3) δ 176.33, 164.24, 163.76, 163.28, 150.17, 148.34, 142.24, 137.17, 132.94, 129.00, 128.73, 116.32, 113.96, 113.29, 61.57, 55.17, 42.86, 39.17, 14.24; IR (diffuse reflectance) 1965, 1727, 1663, 1609, 1568, 1542, 1514, 1493, 1466, 1390, 1297, 1260, 1141, 813, 799, cm−1; MS (EI) m/z 429 (M+), 431, 430, 429, 289, 263, 262, 261, 159, 140, 77; Anal. calcd for C21H20ClN3O5: C, 58.68; H, 4.69; N, 9.77; Cl, 8.25. Found: C, 58.39; H, 4.70; N, 9.71.

後処理

  1. customThe bomb is flushed with CO (3×)
  2. customthe resulting reaction
  3. temperaturecooled to room temperature
  4. washThe organic is washed with water, 1N HCl, brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue is purified by silica gel chromatography (CH2Cl2/MeOH 1/0, 45/1)
  9. customtriturated with MeOH

出典と根拠

ORDレコード
ord-204eac024b4d410fa70ab1f7823c67c4
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06451811B2

反応ノート

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