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Acetic Acid → (E)-7-[2-cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-3,5-dioxo-hept-6-enoic acid diethyl amide

HRID 1072291
ノート
印刷プレビュー

反応式

HRID 1072291 の反応式
[H-].[Na+].C([CH:5](CC)[C:6](=[O:11])[CH2:7][C:8]([NH2:10])=[O:9])C.[CH2:14]([Li])[CH2:15]CC.[CH:19]1([C:22]2[C:31]([CH:32]=[CH:33][C:34](N(OC)C)=[O:35])=[C:30]([C:40]3[CH:45]=[CH:44][C:43]([F:46])=[CH:42][CH:41]=3)[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[N:23]=2)[CH2:21][CH2:20]1.[C:47](O)(=O)[CH3:48].[Na+].[Cl-]>O1CCCC1.O>[CH2:14]([N:10]([CH2:47][CH3:48])[C:8](=[O:9])[CH2:7][C:6](=[O:11])[CH2:5][C:34](=[O:35])/[CH:33]=[CH:32]/[C:31]1[C:22]([CH:19]2[CH2:20][CH2:21]2)=[N:23][C:24]2[C:29]([C:30]=1[C:40]1[CH:41]=[CH:42][C:43]([F:46])=[CH:44][CH:45]=1)=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH3:15]
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

9

反応物 6

HCID 176Acetic AcidHCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 23617702Diethyl acetoacetamideHCID 542239083-[2-cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-N-methoxy-N-methyl-acrylamideHCID 178418339Butyllithium

生成物 1

HCID 20805107
(E)-7-[2-cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-3,5-dioxo-hept-6-enoic acid diethyl amide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒4 回

反応条件

温度
-2.5 °C

実験手順

To a suspension of sodium hydride (600 mg, 25.0 mmol) in tetrahydrofurane (20 ml) under argon is added at −5° C. diethyl acetoacetamide (3.93 g, 25.0 mmol) in tetrahydrofurane (2.0 ml), tetrahydrofurane (22.0 ml), butyllithium (n-heptane solution, 9.2 ml, 25.0 mmol), and a solution of 3-[2-cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-N-methoxy-N-methyl-acrylamide (4.51 g, 12.0 mmol) in tetrahydrofurane (40 ml). After 1 h stirring at −5 to 0° C., acetic acid (4.4 g, 73.3 mmol), 25% aq. NaCl (10 ml), and water (10 ml) are added to the reaction mixture and the mixture is stirred vigorously for 10 min. The (upper) organic phase is washed with 25% aq. NaCl (2×20 ml), the water phases are extracted with ethylacetate (25 ml) and the combined organic phases filtered and evaporated to dryness under reduced pressure. The residue is purified by silica gel chromatography (hexane/ethyl acetate 1:1) to give (E)-7-[2-cyclopropyl-4-(4-fluoro-phenyl)-quinolin-3-yl]-3,5-dioxo-hept-6-enoic acid diethyl amide. Mp. 97-105° C., MS (ES): [M+H]+ 473.

後処理

  1. stirringthe mixture is stirred vigorously for 10 min
  2. washThe (upper) organic phase is washed with 25% aq. NaCl (2×20 ml)
  3. extractionthe water phases are extracted with ethylacetate (25 ml)
  4. filtrationthe combined organic phases filtered
  5. customevaporated to dryness under reduced pressure
  6. customThe residue is purified by silica gel chromatography (hexane/ethyl acetate 1:1)

出典と根拠

ORDレコード
ord-2e94bceb73914c0d8e2cb418bedd88d7
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06909003B2

反応ノート

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