Potassium Carbonate → HCID 59686845, 화합물

HRID 426111노트

반응식

HRID 426111 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 59686845HCID 59686845, 화합물수율 35.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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))

출처 및 근거

ORD 기록
ord-1bf414a94066419097343c9bbe373d44
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106064B2

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