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Cesium carbonate → 6-bromo-3-(2-ethylmorpholino)-N-(4-methoxybenzyl)quinolin-2-amine

HRID 1028972
ノート
印刷プレビュー

反応式

HRID 1028972 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[C:6](I)=[CH:5]2.[CH2:23]([CH:25]1[O:30][CH2:29][CH2:28][NH:27][CH2:26]1)[CH3:24].C(=O)([O-])[O-].[Cs+].[Cs+].C(C1CCCCC1=O)(=O)C(C)C>CN(C=O)C.[Cu]I>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[C:6]([N:27]1[CH2:28][CH2:29][O:30][CH:25]([CH2:23][CH3:24])[CH2:26]1)=[CH:5]2
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

7

反応物 4

HCID 10796Cesium carbonateHCID 114693012-(2-Methylpropanoyl)cyclohexan-1-oneHCID 149332062-EthylmorpholineHCID 673456526-bromo-3-iodo-N-(4-methoxybenzyl)quinolin-2-amine

生成物 1

HCID 712532616-bromo-3-(2-ethylmorpholino)-N-(4-methoxybenzyl)quinolin-2-amine

試薬・触媒・溶媒 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
125 °C

実験手順

A mixture of 6-bromo-3-iodo-N-(4-methoxybenzyl)quinolin-2-amine (0.30 g, 0.640 mmol, prepared as in Example 1, Step 1-2), 2-ethylmorpholine (1.105 g, 9.59 mmol), copper(I) iodide (6.09 mg, 0.032 mmol), cesium carbonate (0.417 g, 1.279 mmol), and 2-isobutyrylcyclohexanone (0.021 mL, 0.128 mmol) in DMF (3 mL) was heated at 125° C. for 10 min. Some product was observed but mostly starting material. The mixture was heated again at 125° C. for 10 min more. This process was repeated 3× until the starting material was completely consumed. The reaction was brought to RT, poured into water (20 mL) and extracted with EtOAc. The combined organics were dried over Na2SO4, filtered, concentrated, and chromatographed on silica gel using gradient 2:1 hexanes/EtOAc to afford a brown oil as 6-bromo-3-(2-ethylmorpholino)-N-(4-methoxybenzyl)quinolin-2-amine.

後処理

  1. temperatureThe mixture was heated again at 125° C. for 10 min more
  2. customwas completely consumed
  3. customwas brought to RT
  4. additionpoured into water (20 mL)
  5. extractionextracted with EtOAc
  6. dry with materialThe combined organics were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customchromatographed on silica gel using gradient 2:1 hexanes/EtOAc

出典と根拠

ORDレコード
ord-25fb7f4caf964db3946e1685e7ddeeb0
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735384B2

反応ノート

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