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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
ノート
印刷プレビュー

反応式

HRID 1675942 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-664836915f4244e2a70a2bc5207a80b1
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08003797B2

反応ノート

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