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Potassium Phosphate, Tribasic → 2-(2,6-Difluorophenyl)-5-(4-morpholinophenylamino)oxazole-4-carbonitrile

HRID 1410479
ノート
印刷プレビュー

反応式

HRID 1410479 の反応式
Br[C:2]1[O:6][C:5]([C:7]2[C:12]([F:13])=[CH:11][CH:10]=[CH:9][C:8]=2[F:14])=[N:4][C:3]=1[C:15]#[N:16].[O:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][CH:24]=2)[CH2:19][CH2:18]1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>CN(C=O)C.CCOC(C)=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:14][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]([F:13])[C:7]=1[C:5]1[O:6][C:2]([NH:27][C:26]2[CH:25]=[CH:24][C:23]([N:20]3[CH2:21][CH2:22][O:17][CH2:18][CH2:19]3)=[CH:29][CH:28]=2)=[C:3]([C:15]#[N:16])[N:4]=1
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 3

HCID 62657Potassium Phosphate, TribasicHCID 75655Benzenamine, 4-(4-morpholinyl)-HCID 595875125-Bromo-2-(2,6-difluorophenyl)oxazole-4-carbonitrile

生成物 1

HCID 595874532-(2,6-Difluorophenyl)-5-(4-morpholinophenylamino)oxazole-4-carbonitrile収率 26%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
180 °C

実験手順

A solution of palladium acetate (0.0057 g, 0.025 mmol) and (±)-2,2″-bis(diphenylphosphino)-1,1″-binaphthalene (0.015 g, 0.024 mmol) in DMF (7.1 mL) was stirred at room temperature for 3 minutes. Then 5-bromo-2-(2,6-difluorophenyl)oxazole-4-carbonitrile (0.100 g, 0.35 mmol), 4-morpholinoaniline (0.250 g, 1.40 mmol) and potassium phosphate tribasic (0.149 g, 0.70 mmol) were added and the mixture heated in the microwave for 3 minutes at 180° C. The reaction was diluted with EtOAc and washed with water. The organic phase was passed through a MP-SH resin cartridge, dried over MgSO4 and the solvent removed in vacuo. The residue was purified by silica gel column chromatography using a gradient 10-100% EtOAc in hexanes to afford 2-(2,6-difluorophenyl)-5-(4-morpholinophenylamino)oxazole-4-carbonitrile (0.035 g, 0.09 mmol, 26%) as an off white solid. 1H NMR (DMSO) δ 3.08 (4H, t), 3.74 (4H, t), 6.97 (2H, d), 7.24 (2H, d), 7.33 (2H, t), 7.64 (1H, m), 10.58 (1H, s). LCMS (2) Rt: 2.92 min; m/z (ES+) 383.

後処理

  1. washwashed with water
  2. dry with materialdried over MgSO4
  3. customthe solvent removed in vacuo
  4. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-60aa87c2a64547ca9f61ba0ae423eb12
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921544B2

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