Triethylamine → HCID 68528893、化合物

HRID 884120ノート

反応式

HRID 884120 の反応式
C(N(CC)CC)C.[NH2:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][C:16]2[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:18][CH:17]=2)=[N:13][CH:14]=1.[Cl:29][C:30]1[CH:31]=[C:32](B(O)O)[CH:33]=[CH:34][C:35]=1[Cl:36]>ClCCl.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[Cl:29][C:30]1[CH:31]=[C:32]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([O:15][C:16]3[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:18][CH:17]=3)=[N:13][CH:14]=2)[CH:33]=[CH:34][C:35]=1[Cl:36]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 27343303,4-Dichlorobenzeneboronic acidHCID 68528473HCID 68528473、化合物

生成物 1

HCID 68528893HCID 68528893、化合物

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (1.2 mL, 8.4 mmol) was added to a suspension of ethyl 3-(4-(5-aminopyridin-2-yloxy)phenyl)propionate (1.2 g, 4.2 mmol), 3,4-dichlorophenylboronic acid (1.6 g, 8.4 mmol), anhydrous copper acetate (0.762 g, 4.2 mmol) and molecular sieves 4A (5 g) in dichloromethane (24 mL), and the resulting reaction solution was stirred overnight at room temperature. After the resulting solution was filtered through Celite, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (n-hexane:ethyl acetate=4:1), to thereby yield 1.5 g of the title compound.

後処理

  1. customthe resulting reaction solution
  2. filtrationAfter the resulting solution was filtered through Celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by silica gel chromatography (n-hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-421fb7f38ea448e6ac6f4ff4d09bc307
出典データセット
uspto-grants-2012_08
特許番号
US08236826B2

反応ノート

読み込み中…