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Triethylamine → N-{4-[6-(3-Bromo-5-methyl-benzoyl)-5-isopropyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl]-pyridin-2-yl}-acetamide

HRID 426159
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HRID 426159 반응식
O[CH2:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH:9][C:10](=[O:12])[CH3:11])[CH:4]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.[Br:25][C:26]1[CH:27]=[C:28]([CH:42]=[C:43]([CH3:45])[CH:44]=1)[C:29]([C:31]1[NH:36][C:35](=[O:37])[NH:34][C:33](=[O:38])[C:32]=1[CH:39]([CH3:41])[CH3:40])=[O:30].C(=O)([O-])[O-].[K+].[K+].[I-].[Li+]>C(Cl)(Cl)Cl.CN(C=O)C>[Br:25][C:26]1[CH:27]=[C:28]([CH:42]=[C:43]([CH3:45])[CH:44]=1)[C:29]([C:31]1[N:36]([CH2:2][C:3]2[CH:8]=[CH:7][N:6]=[C:5]([NH:9][C:10](=[O:12])[CH3:11])[CH:4]=2)[C:35](=[O:37])[NH:34][C:33](=[O:38])[C:32]=1[CH:39]([CH3:40])[CH3:41])=[O:30]
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참가 물질

9

반응물 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 66321Lithium iodideHCID 23151114N-(4-(hydroxymethyl)pyridin-2-yl)acetamideHCID 577518946-(3-bromo-5-methylbenzoyl)-5-isopropylpyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 66705545
N-{4-[6-(3-Bromo-5-methyl-benzoyl)-5-isopropyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl]-pyridin-2-yl}-acetamide
수율 47%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매

실험 절차

N-(4-Hydroxymethyl-pyridin-2-yl)-acetamide (166 mg, 1 mmol) was dissolved in chloroform (10 ml) and cooled in an ice bath under nitrogen atmosphere. With stirring, triethylamine (210 μl, 1.5 mmol) was added and methanesulfonyl chloride (90 μl, 1.2 mmol) was added dropwise. After stirring for 1.1 hr., the reaction mixture was washed with saturated aqueous sodium bicarbonate, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was further dried in high vacuo for ca. 20 min. and mixed with 6-(3-Bromo-5-methyl-benzoyl)-5-isopropyl-1H-pyrimidine-2,4-dione (28) (351 mg, 1 mmol), powdered anhydrous potassium carbonate (138 mg, 1 mmol), and lithium iodide (134 mg, 1 mmol). DMF (5 ml) was then added to the mixture at room temperature and stirred for ca. 4 hr. After evaporation of DMF, the residue was dissolved in methanol-chloroform (1:9) and filtered through celite pad. The filtrate was then evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA:hexanes (2:1); Rf˜0.2 fraction was collected.) to afford 234 mg (47%) of a white solid.

후처리

  1. temperaturecooled in an ice bath under nitrogen atmosphere
  2. stirringAfter stirring for 1.1 hr
  3. wash, the reaction mixture was washed with saturated aqueous sodium bicarbonate
  4. dry with materialdried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe residue was further dried in high vacuo for ca. 20 min.
  8. stirringstirred for ca. 4 hr
  9. customAfter evaporation of DMF
  10. dissolutionthe residue was dissolved in methanol-chloroform (1:9)
  11. filtrationfiltered through celite pad
  12. customThe filtrate was then evaporated in vacuo
  13. customthe residue was purified by silica gel column chromatography (eluent, EA:hexanes (2:1); Rf˜0.2 fraction was collected.)

출처 및 근거

ORD 기록
ord-42f4341aabb3479a8f1ac2147c031aef
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106064B2

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