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Cesium carbonate → 2-(6-(4-isopropylpiperazin-1-yl)-5-methoxypyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one

HRID 1519429
ノート
印刷プレビュー

反応式

HRID 1519429 の反応式
Br[C:2]1[N:7]=[C:6]([C:8]2[NH:17][C:16](=[O:18])[C:15]3[C:10](=[CH:11][C:12]([O:21][CH3:22])=[CH:13][C:14]=3[O:19][CH3:20])[N:9]=2)[CH:5]=[CH:4][C:3]=1[O:23][CH3:24].[CH:25]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)([CH3:27])[CH3:26].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.C([O-])([O-])=O.[Cs+].[Cs+]>ClCCl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH:25]([N:28]1[CH2:33][CH2:32][N:31]([C:2]2[N:7]=[C:6]([C:8]3[NH:17][C:16](=[O:18])[C:15]4[C:10](=[CH:11][C:12]([O:21][CH3:22])=[CH:13][C:14]=4[O:19][CH3:20])[N:9]=3)[CH:5]=[CH:4][C:3]=2[O:23][CH3:24])[CH2:30][CH2:29]1)([CH3:27])[CH3:26]
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 780131-IsopropylpiperazineHCID 634876Binap, (A+-)-HCID 1364081352-(6-bromo-5-methoxypyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one

生成物 1

HCID 1362488532-(6-(4-isopropylpiperazin-1-yl)-5-methoxypyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one収率 25%

試薬・触媒・溶媒 2

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

反応条件

温度
100 °C

実験手順

To a mixture of 2-(6-bromo-5-methoxypyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one (0.196 g, 0.50 mmol), 1-isopropylpiperazine (0.077 g, 0.60 mmol), BINAP (0.062 g, 0.10 mmol), and Cs2CO3 (0.652 g, 2.0 mmol) in nitrogen saturated dioxane (10 mL) was added palladium(II) acetate (0.022 g, 0.10 mmol). The resulting mixture was heated at 100° C. for 3 h. After that time the reaction was cooled to rt, diluted with dichloromethane (100 mL) and washed with water (20 mL). The organic phase was dried over Na2SO4 and concentrated under reduced pressure. The product was purified by flash column chromatography (silica gel, 90:10:0.1 dichloromethane/methanol/ammonium hydroxide) to give 2-(6-(4-isopropylpiperazin-1-yl)-5-methoxypyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one (0.055 g, 25%) as a pale yellow solid: mp 208-210° C.; 1H NMR (400 MHz, CDCl3): δ 10.23 (br s, 1H), 8.08 (d, J=8.0 Hz, 1H), 7.17 (d, J=8.0 Hz, 1H), 6.79 (d, J=2.4 Hz, 1H), 6.45 (d, J=2.4 Hz, 1H), 3.98 (s, 3H), 3.95 (s, 3H), 3.93 (s, 3H), 3.56 (br s, 4H), 2.78 (br s, 5H), 1.15 (d, J=5.6 Hz, 6H); ESI MS m/z 440 [M+H]+.

後処理

  1. temperatureAfter that time the reaction was cooled to rt
  2. washwashed with water (20 mL)
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customThe product was purified by flash column chromatography (silica gel, 90:10:0.1 dichloromethane/methanol/ammonium hydroxide)

出典と根拠

ORDレコード
ord-9b5e15b509e1421b81c53dd47a10f7ef
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073878B2

反応ノート

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