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Cesium fluoride → Methyl 3-amino-2,6-bis(4-methoxyphenyl)isonicotinate

HRID 2410678
ノート
印刷プレビュー

反応式

HRID 2410678 の反応式
[NH2:1][C:2]1[C:11](Br)=[N:10][C:9](Br)=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH3:14][O:15][C:16]1[CH:21]=[CH:20][C:19](B(O)O)=[CH:18][CH:17]=1.[F-].[Cs+]>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[NH2:1][C:2]1[C:11]([C:19]2[CH:20]=[CH:21][C:16]([O:15][CH3:14])=[CH:17][CH:18]=2)=[N:10][C:9]([C:19]2[CH:20]=[CH:21][C:16]([O:15][CH3:14])=[CH:17][CH:18]=2)=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]
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

5

反応物 3

HCID 25953Cesium fluorideHCID 201262(4-Methoxyphenyl)boronic acidHCID 53419616Methyl 3-amino-2,6-dibromoisonicotinate

生成物 1

HCID 66604440Methyl 3-amino-2,6-bis(4-methoxyphenyl)isonicotinate収率 44%

試薬・触媒・溶媒 1

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒

反応条件

温度
80 °C

実験手順

A mixture of methyl 3-amino-2,6-dibromoisonicotinate (500 mg, 1.61 mmol), 4-methoxyphenylboronic acid (588 mg, 3.87 mmol), Tetrakis(triphenylphosphine)-palladium(0) (93 mg, 0.081 mmol) and cesium fluoride (1176 mg, 7.74 mmol) was placed in a vial and flushed with nitrogen. Dimethoxyethane (10 mL) was added and the reaction was heated at 80° C. for 48 hr. After cooling to room temperature, the reaction was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The organic phase was separated, washed with saturated aqueous sodium bicarbonate solution, brine, and then dried with sodium sulfate. Removal of the solvent followed by silica gel radial chromatography (step gradient elution with hexane containing 0 to 25% ethyl acetate) afforded methyl 3-amino-2,6-bis(4-methoxyphenyl)isonicotinate (258 mg, 0.708 mmol, 43.9% yield) as a yellow oil. MS (ESI) m/z 365.2 (M+H). 1H NMR (CDCl3) δ ppm 8.01 (1H, s), 7.91 (2H, d, J=8.85 Hz), 7.66 (2H, d, J=8.55 Hz), 7.02 (2H, d, J=8.55 Hz), 6.94 (2H, d, J=8.85 Hz), 5.93 (2H, br. s.), 3.94 (3H, s), 3.86 (3H, s), 3.83 (3H, s).

後処理

  1. customflushed with nitrogen
  2. additionDimethoxyethane (10 mL) was added
  3. temperatureAfter cooling to room temperature
  4. customthe reaction was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
  5. customThe organic phase was separated
  6. washwashed with saturated aqueous sodium bicarbonate solution, brine
  7. dry with materialdried with sodium sulfate
  8. customRemoval of the solvent
  9. washfollowed by silica gel radial chromatography (step gradient elution with hexane containing 0 to 25% ethyl acetate)

出典と根拠

ORDレコード
ord-173e9b7cdab84842b60fb20333cc1797
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08815840B2

反応ノート

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