Potassium Carbonate → HCID 59686845、化合物

HRID 426111ノート

反応式

HRID 426111 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:18]=[C:19]([CH3:21])[CH:20]=1)[C:5]([C:7]1[NH:12][C:11](=[O:13])[NH:10][C:9](=[O:14])[C:8]=1[CH:15]([CH3:17])[CH3:16])=[O:6].Cl[CH2:23][C:24]1[CH:29]=[C:28]([CH3:30])[N:27]=[C:26]([N:31]2[C:39](=[O:40])[C:38]3[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=3)[C:32]2=[O:41])[CH:25]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Li+]>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH:18]=[C:19]([CH3:21])[CH:20]=1)[C:5]([C:7]1[N:12]([CH2:23][C:24]2[CH:29]=[C:28]([CH3:30])[N:27]=[C:26]([N:31]3[C:39](=[O:40])[C:38]4[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=4)[C:32]3=[O:41])[CH:25]=2)[C:11](=[O:13])[NH:10][C:9](=[O:14])[C:8]=1[CH:15]([CH3:16])[CH3:17])=[O:6]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 66321Lithium iodideHCID 577518946-(3-bromo-5-methylbenzoyl)-5-isopropylpyrimidine-2,4(1H,3H)-dioneHCID 59184674HCID 59184674、化合物

生成物 1

HCID 59686845HCID 59686845、化合物収率 35.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of (28) (351 mg, 1 mmol), (30) (287 mg, 1 mmol), anhydrous powdered potassium carbonate (138 mg, 1 mmol), and lithium iodide (134 mg, 1 mmol), was added DMF (5 ml). The mixture was stirred for overnight at room temperature. The mixture was then evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA: hexanes (from 1:2 to 1:1)) to afford 211 mg (35%) of a white solid; 1H NMR (200 MHz, CDCl3) δ 1.13 (3H, d, J=7.2 Hz), 1.20 (3H, d, J=7.2 Hz), 2.17-2.40 (4H, m), 2.47 (3H, s), 4.49 (1H, d, J=16.0 Hz), 5.15 (1H, d, J=16.0 Hz), 6.84 (1H, s), 6.91 (1H, s), 7.36 (1H, s), 7.53 (1H, s), 7.61 (1H, s), 7.77-7.96 (4H, m), 9.30 (1H, s).

後処理

  1. customThe mixture was then evaporated in vacuo
  2. customthe residue was purified by silica gel column chromatography (eluent, EA: hexanes (from 1:2 to 1:1))

出典と根拠

ORDレコード
ord-1bf414a94066419097343c9bbe373d44
出典データセット
uspto-grants-2012_01
特許番号
US08106064B2

反応ノート

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