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Cesium carbonate → Ethyl 6'-{[(ethylamino)carbonyl]amino}-5''-fluoro-3,3':4',3''-terpyridine-5-carboxylate

HRID 2243033
ノート
印刷プレビュー

反応式

HRID 2243033 の反応式
Br[C:2]1[C:3]([C:14]2[CH:15]=[N:16][CH:17]=[C:18]([F:20])[CH:19]=2)=[CH:4][C:5]([NH:8][C:9]([NH:11][CH2:12][CH3:13])=[O:10])=[N:6][CH:7]=1.CC1(C)C(C)(C)OB([C:29]2[CH:30]=[N:31][CH:32]=[C:33]([CH:39]=2)[C:34]([O:36][CH2:37][CH3:38])=[O:35])O1.C(=O)([O-])[O-].[Cs+].[Cs+]>>[CH2:12]([NH:11][C:9]([NH:8][C:5]1[N:6]=[CH:7][C:2]([C:29]2[CH:30]=[N:31][CH:32]=[C:33]([C:34]([O:36][CH2:37][CH3:38])=[O:35])[CH:39]=2)=[C:3]([C:14]2[CH:15]=[N:16][CH:17]=[C:18]([F:20])[CH:19]=2)[CH:4]=1)=[O:10])[CH3:13]
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

4

反応物 3

HCID 10796Cesium carbonateHCID 3816953Ethyl 5-(tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-3-carboxylateHCID 59208332N-(5'-bromo-5-fluoro-3,4'-bipyridin-2'-yl)-N'-ethylurea2 回

生成物 1

HCID 59208334Ethyl 6'-{[(ethylamino)carbonyl]amino}-5''-fluoro-3,3':4',3''-terpyridine-5-carboxylate収率 46.4%

反応条件

温度
100 °C

実験手順

N-(5′-bromo-5-fluoro-3,4′-bipyridin-2′-yl)-N′-ethylurea (Intermediate 30, 0.34 g, 1.00 mmol), ethyl 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)nicotinate (Oakwood Products, Inc., Cat. #021607) (0.306 g, 1.10 mmol), tetrakis triphenyl phosphine palladium (0.058 g, 0.05 mmol), and cesium carbonate (0.359 g, 1.10 mmol) were added to a microwave vial and degassed with nitrogen. A solution of 1,4-dioxane:water (4:1, 10 mL) was added to the solution and the reaction mixture was heated to 100° C. for 30 minutes. The reaction mixture was partitioned between water and ethyl acetate, and the organic layer was washed with saturated sodium bicarbonate solution, water, and brine, then dried over magnesium sulfate. The solvent was removed and the residue was purified by silica gel chromatography, eluting with (0-100% EtOAc/hexanes) to give the title compound as a white solid (190 mg). MS (ESP): 410 (MH+) for C21H20FN5O3;

後処理

  1. customdegassed with nitrogen
  2. additionA solution of 1,4-dioxane:water (4:1, 10 mL) was added to the solution
  3. customThe reaction mixture was partitioned between water and ethyl acetate
  4. washthe organic layer was washed with saturated sodium bicarbonate solution, water, and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed
  7. customthe residue was purified by silica gel chromatography
  8. washeluting with (0-100% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-2b94de32c4c24cbea31bde6943355beb
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674801B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート