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Imidazole → HCID 22106242、化合物

HRID 1456380
ノート
印刷プレビュー

反応式

HRID 1456380 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].[CH2:14]([N:18]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][N:26]=2)[C:21]([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([O:34][CH2:35][CH2:36][CH2:37]Cl)[CH:29]=2)=[C:20]([NH:39][C:40]([NH:42][C:43]2[C:48]([CH:49]([CH3:51])[CH3:50])=[CH:47][CH:46]=[CH:45][C:44]=2[CH:52]([CH3:54])[CH3:53])=[O:41])[C:19]1=[O:55])[CH2:15][CH2:16][CH3:17]>CN(C=O)C.O>[CH2:14]([N:18]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][N:26]=2)[C:21]([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([O:34][CH2:35][CH2:36][CH2:37][N:1]3[CH:5]=[CH:4][N:3]=[CH:2]3)[CH:29]=2)=[C:20]([NH:39][C:40]([NH:42][C:43]2[C:48]([CH:49]([CH3:51])[CH3:50])=[CH:47][CH:46]=[CH:45][C:44]=2[CH:52]([CH3:53])[CH3:54])=[O:41])[C:19]1=[O:55])[CH2:15][CH2:16][CH3:17]
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 795ImidazoleHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 22105972HCID 22105972、化合物

生成物 1

HCID 22106242HCID 22106242、化合物収率 38.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

To a suspension of imidazole (97 mg, 1.43 mmol), potassium carbonate (246 mg, 1.78 mmol) and sodium iodide (35 mg) in DMF (20 ml) was added N-[1-(butyl-4-{3-(3-chloropropoxy)phenyl}-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N'-(2,6-diisopropylphenyl)urea (700 mg, 1.19 mmol), and the mixture was stirred at 50°-60° C. for 10 hours. After allowed to stand for cooling, the mixture was poured into water, extracted with ethyl acetate, and the extract was washed with water, washed with a saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The residue was concentrated under reduced pressure, and purified by silica gel column chromatography (5% methanol in chloroform) to give the title compound (286 mg, 0.46 mmol).

後処理

  1. temperaturefor cooling
  2. extractionextracted with ethyl acetate
  3. washthe extract was washed with water
  4. washwashed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe residue was concentrated under reduced pressure
  7. custompurified by silica gel column chromatography (5% methanol in chloroform)

出典と根拠

ORDレコード
ord-fa3c43564139407295add8faec42c623
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05843957

反応ノート

読み込み中…

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