Triethylamine → HCID 53921157、化合物

HRID 379038

反応式

HRID 379038 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].[CH:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14][C:13]=1B(O)O.[CH2:25](N(CC)CC)C>C(Cl)Cl>[CH3:25][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([I:11])=[C:2]([O:1][C:13]2[CH:14]=[CH:15][C:16]3[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:12]=2)[CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 7368543-Hydroxy-4-iodobenzoic acidHCID 2734375(Naphthalen-2-yl)boronic acid

生成物 1

HCID 53921157HCID 53921157、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-hydroxy-4-iodo-benzoic acid acid methyl ester (0.505 g, 1.82 mmol), cupric acetate (0.330 g, 1.82 mmol), 2-naphthylboronic acid (0.625 g, 3.63 mmol) and powdered 4A molecular sieves (0.3 g) in CH2Cl2 (21 mL) was treated with triethylamine (1.27 mL, 9.08 mmol) and stirred at ambient temperature for 18 hr. The reaction mixture was filtered through celite, concentrated to dryness and chromatographed (SiO2, 5-40% EtOAc: hexane) to give the title compound. FAB mass spectrum (M+1) 405.

後処理

  1. filtrationThe reaction mixture was filtered through celite,
  2. concentrationconcentrated to dryness
  3. customchromatographed (SiO2, 5-40% EtOAc: hexane)

出典と根拠

ORDレコード
ord-4c3bea01e7014b94b4af9526bf27f2c4
出典データセット
uspto-grants-2001_10
特許番号
US06297239B1

関連ノート

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