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Cesium carbonate → [2-Amino-6-[(4-methylpiperazin-1-yl)methyl]quinazolin-4-yl]-isoindolin-2-ylmethanone

HRID 1400167
ノート
印刷プレビュー

反応式

HRID 1400167 の反応式
[NH2:1][C:2]1[N:11]=[C:10]([C:12]([N:14]2[CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH2:15]2)=[O:13])[C:9]2[C:4](=[CH:5][CH:6]=[C:7](I)[CH:8]=2)[N:3]=1.[B-](F)(F)(F)[CH2:25][N:26]1[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]1.[K+].C(C1C=C(C(C)C)C=C(C(C)C)C=1P(C1CCCCC1)C1CCCCC1)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCCC1.C([O-])(=O)C.C([O-])(=O)C.[Pd+2].O>[NH2:1][C:2]1[N:11]=[C:10]([C:12]([N:14]2[CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH2:15]2)=[O:13])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH2:25][N:26]3[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]3)[CH:8]=2)[N:3]=1
参加物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 9801140Dicyclohexyl(2,4,6-triisopropylphenyl)phosphineHCID 45588174Potassium 1-methyl-4-trifluoroboratomethylpiperazineHCID 58457195(2-Amino-6-iodoquinazolin-4-yl)isoindolin-2-ylmethanone

生成物 1

HCID 52939797[2-Amino-6-[(4-methylpiperazin-1-yl)methyl]quinazolin-4-yl]-isoindolin-2-ylmethanone

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

75 mg of (2-amino-6-iodoquinazolin-4-yl)isoindolin-2-ylmethanone are suspended in 2 ml of tetrahydrofuran and 7 μl of water together with 40 mg of potassium 1-methyl-4-trifluoroboratomethylpiperazine, 1 mg of palladium diacetate, 4 mg of ((2,4,6 triisopropyl)phenyl)dicyclohexylphosphine and 176 mg of caesium carbonate, and the mixture is stirred at 80° C. for 48 h. After cooling, the mixture is filtered through kieselguhr, rinsed three times with 5 ml of tetrahydrofuran each time, and the filtrate is evaporated to dry ness in vacuo. The residue is purified by means of preparative HPLC, and the title compound is isolated.

後処理

  1. temperatureAfter cooling
  2. filtrationthe mixture is filtered through kieselguhr
  3. washrinsed three times with 5 ml of tetrahydrofuran each time
  4. customthe filtrate is evaporated
  5. customto dry ness in vacuo
  6. customThe residue is purified by means of preparative HPLC

出典と根拠

ORDレコード
ord-07ef5567ee444f72a1f3fa442e2dd120
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08906930B2

反応ノート

読み込み中…

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