Dichloromethane → 1~2~,2~2~:2~3~,3~2~-Terpyridine

HRID 25862

反応式

HRID 25862 の反応式
Cl.[C:2](Cl)(=O)[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1.CC[N:13]([CH:17]([CH3:19])C)[CH:14]([CH3:16])C.CO[C:22]1[CH:27]=CC=[C:24]([NH2:28])[CH:23]=1.[CH2:29](Cl)Cl>>[N:13]1[CH:14]=[CH:16][CH:29]=[CH:19][C:17]=1[C:4]1[C:3]([C:2]2[CH:27]=[CH:22][CH:23]=[CH:24][N:28]=2)=[CH:8][CH:7]=[CH:6][N:5]=1

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 108243-MethoxyanilineHCID 81531DiisopropylethylamineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)

生成物 1

HCID 149389711~2~,2~2~:2~3~,3~2~-Terpyridine

実験手順

Nicotinoyl chloride hydrochloride (0.3 g, 1.685 mmol), DIEA (0.65 g, 5.06 mmol, 3.0 eqv), and ortho- or meta-anisidine (0.21 g, 1.68 mmol, 1 eqv) were dissolved in CH2Cl2 and stirred at rt for 48 h. The solution was extracted with 1N HCl solution. The aqueous layer was neutralized with a NaHCO3 solution and extracted with CH2Cl2. The organic extracts were combined, dried (MgSO4), filtered, and concentrated in vacuo to give a white solid.

後処理

  1. extractionThe solution was extracted with 1N HCl solution
  2. extractionextracted with CH2Cl2
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give a white solid

出典と根拠

ORDレコード
ord-cb847d7ade3d49c2ad756e823e9807e5
出典データセット
uspto-grants-2005_02
特許番号
US06858600B2

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