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

HRID 1246728
ノート
印刷プレビュー

反応式

HRID 1246728 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH:11]=[C:10]([C:13]([OH:15])=O)[CH2:9][CH2:8]1.C(Cl)(C(Cl)=O)=O.N1C=CC=CC=1.[C:28]([C:32]1[CH:38]=[CH:37][C:35]([NH2:36])=[CH:34][CH:33]=1)([CH3:31])([CH3:30])[CH3:29]>C(Cl)Cl.C1(C)C=CC=CC=1.CN(C1C=CN=CC=1)C.O.CN(C=O)C>[C:28]([C:32]1[CH:33]=[CH:34][C:35]([NH:36][C:13]([C:10]2[CH2:9][CH2:8][N:7]([C:2]3[N:1]=[CH:6][CH:5]=[CH:4][N:3]=3)[CH2:12][CH:11]=2)=[O:15])=[CH:37][CH:38]=1)([CH3:31])([CH3:29])[CH3:30]
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 219047301-Pyrimidin-2-yl-1,2,3,6-tetrahydropyridine-4-carboxylic acid

生成物 1

HCID 44580004N-(4-tert-Butylphenyl)-1-(pyrimidin-2-yl)-1,2,3,6-tetrahydropyridine-4-carboxamide収率 534.8%

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

To a suspension of 1-Pyrimidin-2-yl-1,2,3,6-tetrahydro-pyridine-4-carboxylic acid (60.4 mg, 0.194 mmol) and DMF (cat) in CH2Cl2 (1 mL) was added (COCl)2 (0.027 mL, 0.31 mmol). The mixture was stirred for 90 minutes, diluted with PhMe (0.5 mL), concentrated under reduced pressure to dryness, and dissolved in CH2Cl2 (1.5 mL). To the solution were added pyridine (0.027 mL, 0.33 mmol), DMAP (cat), and 4-tert-butylaniline (0.037 mL, 0.023 mmol). The mixture was stirred 1 hour, diluted with water and extracted with CH2Cl2, dried (Na2SO4), and purified by flash chromatography (7% EtOAc/CH2Cl2) to provide 1-Pyrimidin-2-yl-1,2,3,6-tetrahydro-pyridine-4-carboxylic acid (4-tert-butyl-phenyl)-amide as a white solid (54.2 mg, 0.123 mmol, 63%): MS (ESI+) m/z 337 (M+H)+, m/z 334 (M−H)−; 1H NMR (300 MHz, CHLOROFORM-D) δ ppm 1.31 (s, 9 H), 2.59 (m, 2 H), 4.04 (t, J=5.6 Hz, 2 H), 4.44 (q, J=3.1 Hz, 2 H), 6.54 (t, J=4.7 Hz, 1 H), 6.75 (m, 1 H), 7.36 (m, 3 H), 7.47 (m, 2 H), 8.35 (d, J=4.7 Hz, 2 H).

後処理

  1. concentrationconcentrated under reduced pressure to dryness
  2. dissolutiondissolved in CH2Cl2 (1.5 mL)
  3. stirringThe mixture was stirred 1 hour
  4. extractionextracted with CH2Cl2
  5. dry with materialdried (Na2SO4)
  6. custompurified by flash chromatography (7% EtOAc/CH2Cl2)

出典と根拠

ORDレコード
ord-832cb8baa5f742c599e05cef6d7cd5c7
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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