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Triethylamine → 1-[2-Chloro-6-(4-methoxy-benzylamino)-pyridin-4-ylmethyl]-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-1H-pyrimidine-2,4-dione

HRID 426214
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HRID 426214 반응식
F[C:2]1[CH:7]=[C:6]([CH2:8]O)[CH:5]=[C:4]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[N:3]=1.C(N(CC)CC)C.CS([Cl:31])(=O)=O.C([O:39][C:40]1[N:45]=[C:44]([O:46]CC2C=CC=CC=2)[C:43]([CH:54]([CH3:56])[CH3:55])=[C:42]([O:57][C:58]2[CH:63]=[C:62]([CH3:64])[CH:61]=[C:60]([CH:65]3[O:69][CH2:68][CH2:67][O:66]3)[CH:59]=2)[N:41]=1)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Li+]>C(Cl)(Cl)Cl.ClCCl.CN(C=O)C>[Cl:31][C:2]1[CH:7]=[C:6]([CH2:8][N:41]2[C:42]([O:57][C:58]3[CH:63]=[C:62]([CH3:64])[CH:61]=[C:60]([CH:65]4[O:69][CH2:68][CH2:67][O:66]4)[CH:59]=3)=[C:43]([CH:54]([CH3:56])[CH3:55])[C:44](=[O:46])[NH:45][C:40]2=[O:39])[CH:5]=[C:4]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[N:3]=1
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참가 물질

10

반응물 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 66321Lithium iodideHCID 59184650HCID 59184650, 화합물HCID 591846532,4-Bis-benzyloxy-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-pyrimidine

생성물 1

HCID 59184794
1-[2-Chloro-6-(4-methoxy-benzylamino)-pyridin-4-ylmethyl]-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-1H-pyrimidine-2,4-dione
수율 57.2%

시약·촉매·용매 3

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 2-fluoro-6-(p-methoxybenzylamino)-4-pyridine-methanol (790 mg, 2.84 mmol) in chloroform (28 ml) at 0° C. (ice bat), was added triethylamine (597 μl, 4.26 mmol) followed by methanesulfonyl chloride (256 μl, 3.41 mmol). After stirring for 1.5 hr., the mixture was diluted with dichloromethane, washed with aqueous saturated sodium bicarbonate solution, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was further dried in high vacuo and mixed with compound 8 (945 mg, 2.84 mmol), anhydrous powdered potassium carbonate (392 mg, 2.84 mmol), and lithium iodide (381 mg, 2.84 mmol). Anhydrous DMF (15 ml) was then added into the mixture and stirred for overnight at room temperature. The mixture was evaporated in vacuo. The residue was dissolved in methanol-dichloromethane (1:9), filtered through a celite pad, and the pad was washed with dichloromethane. The combined filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:2)) to afford 963 mg (57%) of a white foam. 1H NMR (200 MHz, CDCl3) δ 1.11 (6H, d, J=7.0 Hz), 2.30 (3H, s), 2.72 (1H, m), 3.79 (3H, s), 3.93-4.06 (4H, m), 4.30 (2H, d, J=5.4 Hz), 4.67 (2H, s), 5.04 (1H, t, J=5.4 Hz), 5.67 (1H, s), 5.96 (1H, s), 6.36 (1H, s), 6.57 (1H, s), 6.79 (1H, s), 6.85 (2H, d, J=8.4 Hz), 7.01 (1H, s), 7.22 (2H, d, J=8.4 Hz), 9.01 (1H, s).

후처리

  1. washwashed with aqueous saturated sodium bicarbonate solution
  2. dry with materialdried with anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was further dried in high vacuo
  6. stirringstirred for overnight at room temperature
  7. customThe mixture was evaporated in vacuo
  8. dissolutionThe residue was dissolved in methanol-dichloromethane (1:9)
  9. filtrationfiltered through a celite pad
  10. washthe pad was washed with dichloromethane
  11. customThe combined filtrate was evaporated in vacuo
  12. customthe residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:2))

출처 및 근거

ORD 기록
ord-16c7f40ddeb2407181158171f79cfa16
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106064B2

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