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Cesium carbonate → 7-Methoxy-6-(2-methylphenyl)-N-phenylquinazolin-2-amine

HRID 602387
ノート
印刷プレビュー

反応式

HRID 602387 の反応式
[NH2:1][C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][C:6]([O:19][CH3:20])=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[CH:8]=2)[N:3]=1.I[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.CC1(C)C2C=CC=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=2OC2C1=CC=CC=2P(C1C=CC=CC=1)C1C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O>[NH:1]([C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][C:6]([O:19][CH3:20])=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[CH:8]=2)[N:3]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=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

8

反応物 4

HCID 10796Cesium carbonateHCID 11575IodobenzeneHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 670614707-Methoxy-6-(2-methylphenyl)quinazolin-2-amine

生成物 1

HCID 670616607-Methoxy-6-(2-methylphenyl)-N-phenylquinazolin-2-amine収率 85%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

2-Amino-7-methoxy-6-(2-methylphenyl)quinazoline (150 mg, 0.565 mmol) obtained in Example 174 was dissolved in dioxane (5.7 mL) and the solution was added with iodobenzene (70 μL, 0.622 mmol), tris(dibenzylideneacetone)dipalladium (25.9 mg, 0.028 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (36 mg, 0.062 mmol) and cesium carbonate (258 mg, 0.791 mmol), followed by stirring at 100° C. for 20 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, then the solvent was evaporated under reduced pressure. The residue was purified by preparative thin-layer chromatography (ethyl acetate/hexane=3/7) to obtain 2-anilino-7-methoxy-6-(2-methylphenyl)quinazoline (164 mg, 85%). In a similar manner to Example 19, Compound 178 was obtained using the above-obtained 2-anilino-7-methoxy-6-(2-methylphenyl)quinazoline.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by preparative thin-layer chromatography (ethyl acetate/hexane=3/7)

出典と根拠

ORDレコード
ord-dc3b55c38ec544ff8cd657fe4c490e77
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07906522B2

反応ノート

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