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Pyridine → N-(4-tert-Butylphenyl)-1-(3-(trifluoromethyl)pyridin-2-yl)-1,2,3,6-tetrahydropyridine-4-carboxamide

HRID 1246723
ノート
印刷プレビュー

反応式

HRID 1246723 の反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[C:4]([N:9]2[CH2:14][CH:13]=[C:12]([C:15]([OH:17])=O)[CH2:11][CH2:10]2)=[N:5][CH:6]=[CH:7][CH:8]=1.C(Cl)(C(Cl)=O)=O.N1C=CC=CC=1.[C:32]([C:36]1[CH:42]=[CH:41][C:39]([NH2:40])=[CH:38][CH:37]=1)([CH3:35])([CH3:34])[CH3:33]>C(Cl)Cl.C1(C)C=CC=CC=1.CN(C1C=CN=CC=1)C.O.CN(C=O)C>[C:32]([C:36]1[CH:37]=[CH:38][C:39]([NH:40][C:15]([C:12]2[CH2:11][CH2:10][N:9]([C:4]3[C:3]([C:2]([F:1])([F:19])[F:18])=[CH:8][CH:7]=[CH:6][N:5]=3)[CH2:14][CH:13]=2)=[O:17])=[CH:41][CH:42]=1)([CH3:35])([CH3:33])[CH3:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 1049PyridineHCID 65578Oxalyl chlorideHCID 698614-Tert-ButylanilineHCID 21904722HCID 21904722、化合物

生成物 1

HCID 11407011N-(4-tert-Butylphenyl)-1-(3-(trifluoromethyl)pyridin-2-yl)-1,2,3,6-tetrahydropyridine-4-carboxamide

試薬・触媒・溶媒 5

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 6228Dimethylformamide溶媒
HCID 6344Dichloromethane溶媒

実験手順

3′-(Trifluoromethyl)-3,6-dihydro-2H-1,2′-bipyridine-4-carboxylic acid (0.300 g, 1.10 mmol) and a catalytic amount of DMF were combined in CH2Cl2 (4.0 mL) and treated with (COCl)2 (0.14 mL, 1.6 mmol). The mixture was stirred for 90 minutes, diluted with toluene (0.5 mL) and concentrated to dryness. The residue was dissolved in CH2Cl2 (4.0 mL) treated with pyridine (0.14 mL, 1.7 mmol), a catalytic amount of DMAP, and 4-tert-butylaniline (0.21 mL, 1.3 mmol). After 1 hour, the mixture was diluted with water and extracted with CH2Cl2. The organic phase was dried (Na2SO4), filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography (2.5% ethyl acetate/CH2Cl2) to provide the title compound. 1H NMR (300 MHz, CDCl3) δ 8.42 (dd, 1H), 7.89 (dd, 1H), 7.47 (d, 3H), 6.98 (dd, 1H), 6.76 (s, 1H), 4.06 (q, 2H), 3.53 (t, 2H), 2.67 (m, 2H); MS (m/z) 404.

後処理

  1. concentrationconcentrated to dryness
  2. dissolutionThe residue was dissolved in CH2Cl2 (4.0 mL)
  3. waitAfter 1 hour
  4. extractionextracted with CH2Cl2
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe residue was purified by flash chromatography (2.5% ethyl acetate/CH2Cl2)

出典と根拠

ORDレコード
ord-b25e0cfbe1244753aa56bb7026b73529
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07129235B2

反応ノート

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