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1,2-Dichloroethane → N-[(5,6-dimethoxy-2-pyridinyl)methyl]-2-(3-fluorophenyl)-5-(5-methyl-3-pyridinyl)pyridine-3-carboxamide

HRID 1675942
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HRID 1675942 반응식
Cl.[F:2][C:3]1[CH:4]=[C:5]([C:9]2[N:14]=[CH:13][C:12]([C:15]3[CH:16]=[N:17][CH:18]=[C:19]([CH3:21])[CH:20]=3)=[CH:11][C:10]=2[C:22](O)=[O:23])[CH:6]=[CH:7][CH:8]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[CH3:39][O:40][C:41]1[CH:42]=[CH:43][C:44]([CH2:49][NH2:50])=[N:45][C:46]=1[O:47][CH3:48].CN1CCOCC1>CN(C)C=O>[CH3:39][O:40][C:41]1[CH:42]=[CH:43][C:44]([CH2:49][NH:50][C:22]([C:10]2[CH:11]=[C:12]([C:15]3[CH:16]=[N:17][CH:18]=[C:19]([CH3:21])[CH:20]=3)[CH:13]=[N:14][C:9]=2[C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([F:2])[CH:4]=2)=[O:23])=[N:45][C:46]=1[O:47][CH3:48]
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참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 574847121-(5,6-Dimethoxypyridin-2-yl)methanamineHCID 673474386-(3-Fluorophenyl)-5'-methyl-3,3'-bipyridine-5-carboxylic acid hydrochloride

생성물 1

HCID 25225521
N-[(5,6-dimethoxy-2-pyridinyl)methyl]-2-(3-fluorophenyl)-5-(5-methyl-3-pyridinyl)pyridine-3-carboxamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
0 °C

실험 절차

To a solution of 6-(3-fluorophenyl)-5′-methyl-3,3′-bipyridine-5-carboxylic acid hydrochloride (3-6, prepared by the method described above for the preparation of 3-4, 2.5 g, 7.25 mmol) in dimethylformamide (36 mL) cooled to 0° C., was added EDC (1.95 g, 10.2 mmol) and HOBt (1.67 g, 10.9 mmol) followed by 1-(5,6-dimethoxypyridin-2-yl)methanamine (11-6, 1.46 g, 8.7 mmol) and N-methylmorpholine (4.78 mL, 43.5 mmol). The reaction stirred for 15 minutes and then was allowed to warm to room temperature. After 3.5 hours the reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate. The organics were washed with water and brine, dried over Na2SO4/MgSO4, filtered and stripped to dryness. The crude product was recrystallized from chloroform/ethyl ether to afford the title compound (3-7) as a white solid. 1H NMR (500 MHz, CDCl3) δ 8.96 (d, J=2.2 Hz, 1H), 8.72 (d, J=1.7 Hz, 1H), 8.56 (s, 1H), 8.23 (d, J=2.2 Hz, 1H), 7.76 (s, 1H), 7.44 (d, J=7.8 Hz, 1H), 7.40 (d, J=9.5 Hz, 1H), 7.24 (m, 1H), 6.99 (m, 2H), 6.74 (d, J=7.8 Hz, 1H), 6.33 (m, 1H), 4.44 (d, J=5.4 Hz, 2H), 3.88 (s, 3H), 3.76(s, 3H), 2.45 (s, 3H). HRMS [M+H] C26H23FN4O3 calc'd 459.1827, found 459.1832.

후처리

  1. temperatureto warm to room temperature
  2. customAfter 3.5 hours the reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate
  3. washThe organics were washed with water and brine
  4. dry with materialdried over Na2SO4/MgSO4
  5. filtrationfiltered
  6. customThe crude product was recrystallized from chloroform/ethyl ether

출처 및 근거

ORD 기록
ord-664836915f4244e2a70a2bc5207a80b1
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08003797B2

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